United States
Environmental Protection
Agency
Office of Air Quality
Planning and Standards
Research Triangle Park, NC 27711
EPA-454/R-00-014
April 2000
AIR
&EPA
Final Report
Manual Testing
Lime Kiln No. 1
Scrubber Inlet and Stack
Chemical Lime Company
Alabaster, Alabama
c of Air
Clean
-i_ ;*
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FINAL REPORT
MANUAL TESTING
LIME KILN NO. 1 SCRUBBER INLET AND STACK
CHEMICAL LIME COMPANY
ALABASTER, ALABAMA
EPA Contract No. 68-D-98-004
Work Assignment No. 3-03
Prepared for:
Mr. Michael L. Toney (MD-19)
Work Assignment Manager
SCGA, EMC, OAQPS
U.S. Environmental Protection Agency
Research Triangle Park, NC 27711
April 2000
P:\S523\FINRPTS\ALABAST\FINAL.WPD
Submitted by
PACIFIC ENVIRONMENTAL SERVICES, INC.
5001 S. Miami Blvd., Suite 300
Post Office Box 12077
Research Triangle Park, NC 27709-2077
(919) 941-0333
FAX (919) 941-0234 U.S. Environmental Protection Agenc,
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DISCLAIMER
This document was prepared by Pacific Environmental Services, Inc. (PES) under EPA
Contract No. 68-D98-004, Work Assignment No. 3-03. This document has been reviewed
following PES' internal quality assurance procedures and has been approved for distribution. The
contents of this document do not necessarily reflect the views and policies of the U.S.
Environmental Protection Agency (EPA). Mention of trade names does not constitute
endorsement by the EPA or PES.
11
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TABLE OF CONTENTS
Page
1.0 INTRODUCTION 1-1
2.0 SUMMARY OF RESULTS 2-1
2.1 EMISSIONS TEST LOG 2-1
2.2 PCDDs/PCDFs 2-2
2.3 HYDROGEN CHLORIDE, AMMONIA, AND CATIONS 2-3
3.0 PROCESS DESCRIPTION 3-1
4.0 SAMPLING LOCATIONS 4-1
4.1 KILNNO. 1 SCRUBBER INLET 4-1
4.2 KILNNO. 1 SCRUBBER STACK 4-1
5.0 SAMPLING AND ANALYTICAL PROCEDURES 5-1
5.1 LOCATION OF MEASUREMENT SITES AND
SAMPLE/VELOCITY TRAVERSE POINTS 5-1
5.2 DETERMINATION OF EXHAUST GAS VOLUMETRIC
FLOW RATE 5-2
5.3 DETERMINATION OF EXHAUST GAS MOISTURE CONTENT 5-3
5.4 DETERMINATION OF PCDDs/PCDFs 5-3
5.5 DETERMINATION OF HYDROGEN CHLORIDE, AMMONIA,
AND CATIONS 5-4
5.6 DETERMINATION OF CARBON DIOXIDE, OXYGEN, TOTAL
HYDROCARBONS, AND HYDROGEN CHLORIDE 5-7
6.0 QUALITY ASSURANCE/QUALITY CONTROL PROCEDURES AND RESULTS 6-1
6.1 CALIBRATION OF APPARATUS 6-1
6.2 ON-SITE MEASUREMENTS 6-4
6.3 LABORATORY ANALYSES 6-5
111
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TABLE OF CONTENTS (Concluded)
APPENDIX A RAW FIELD DATA
APPENDIX A. 1 RAW FIELD DATA, KILN NO. 1 SCRUBBER INLET
APPENDIX A.2 RAW FIELD DATA, KILN NO. 1 SCRUBBER OUTLET
APPENDIX B LABORATORY ANALYTICAL DATA
APPENDIX B. 1 LABORATORY ANALYTICAL DATA, METHOD 26A
APPENDIX B.2 LABORATORY ANALYTICAL DATA, METHOD 23
APPENDIX C
APPENDIX D
APPENDIX E
APPENDIX F
APPENDIX G
CALCULATIONS
CALIBRATION DATA
PARTICIPANTS
PROCESS DATA
TEST METHODS
IV
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LIST OF TABLES
Page
TABLE 2.1 EMISSIONS TEST LOG, CHEMICAL LIME COMPANY - ALABASTER,
ALABAMA 2-1
TABLE 2.2 PCDDS/PCDFS SAMPLING AND EXHAUST GAS PARAMETERS,
KILN NO. 1 SCRUBBER INLET AND STACK, CHEMICAL LIME
COMPANY - ALABASTER, ALABAMA 2-4
TABLE 2.3 PCDDS/PCDFS CONCENTRATIONS AND EMISSION RATES,
KILN NO. 1 SCRUBBER INLET AND STACK, CHEMICAL LIME
COMPANY - ALABASTER, ALABAMA 2-5
TABLE 2.4 PCDDS/PCDFS CONCENTRATIONS AND 2378-TCDD TOXIC
EQUIVALENT CONCENTRATIONS ADJUSTED TO 7 PERCENT
OXYGEN, KILN NO. 1 SCRUBBER INLET AND STACK,
CHEMICAL LIME COMPANY - ALABASTER, ALABAMA 2-6
TABLE 2.5 HCL AND AMMONIA SAMPLING AND EXHAUST GAS PARAMETERS,
KILN NO. 1 SCRUBBER INLET, CHEMICAL LIME COMPANY -
ALABASTER, ALABAMA 2-7
TABLE 2.6 HCL, AMMONIA, AND CATIONS CONCENTRATIONS AND
EMISSION RATES, KILN NO. 1 SCRUBBER INLET, CHEMICAL LIME
COMPANY - ALABASTER, ALABAMA 2-8
TABLE 2.7 HCL AND AMMONIA SAMPLING AND EXHAUST GAS PARAMETERS,
KILN NO. 1 SCRUBBER OUTLET, CHEMICAL LIME COMPANY -
ALABASTER, ALABAMA 2-9
TABLE 2.8 HCL, AMMONIA, AND CATIONS CONCENTRATIONS AND
EMISSION RATES, KILN NO. 1 SCRUBBER OUTLET, CHEMICAL
LIME COMPANY - ALABASTER, ALABAMA 2-10
TABLE 5.1 SUMMARY OF SAMPLING LOCATIONS, TEST PARAMETERS,
SAMPLING LOCATIONS, AND NUMBER AND DURATION OF
TESTS, CHEMICAL LIME COMPANY, ALABASTER, ALABAMA 5-2
TABLE 6.1 SUMMARY OF TEMPERATURE SENSOR CALIBRATION DATA 6-2
TABLE 6.2 SUMMARY OF PITOT TUBE DIMENSIONAL DATA 6-3
TABLE 6.3 SUMMARY OF DRY GAS METER AND ORIFICE
CALIBRATION DATA 6-4
TABLE 6.4 SUMMARY OF EPA METHODS 23 AND 26A FIELD
SAMPLING QA/QC DATA 6-6
TABLE 6.5 SUMMARY OF EPA METHOD 23 STANDARDS RECOVERY
EFFICIENCIES 6-8
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LIST OF TABLES (Concluded)
TABLE 6.6 SUMMARY OF EPA METHOD 26A LABORATORY ANALYSIS
QC DATA, ANION SPIKES, AND DUPLICATES 6-9
TABLE 6.7 SUMMARY OF EPA METHOD 26A LABORATORY ANALYSIS
QC DATA, CATION SPIKES, AND DUPLICATES 6-10
TABLE 6.8 SUMMARY OF EPA METHOD 26A ANALYSIS FIELD BLANK
RESULTS 6-11
VI
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LIST OF FIGURES
Page
Figure 1.1 Key Personnel and Responsibility for Field Testing at Chemical Lime
Company - Alabaster, Alabama 1-3
Figure 4.1 Kiln No. 1 Process Flow Schematic Showing Testing Locations, Chemical
Lime Company - Alabaster, Alabama 4-3
Figure 4.2 Kiln No. 1 Scrubber Inlet Test Location and Traverse Point Locations,
Chemical Lime Company - Alabaster, Alabama 4-4
Figure 4.3 Kiln No. 1 Scrubber Stack Test Location and Traverse Point Locations,
Chemical Lime Company - Alabaster, Alabama 4-5
Figure 5.1 Sampling Train Schematic for EPA Method 23 5-5
Figure 5.2 Sampling Train Schematic for EPA Method 26A 5-6
Vll
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1.0 INTRODUCTION
The U.S. Environmental Protection Agency (EPA) Emission Standards Division (ESD) is
investigating the lime manufacturing industry to identify and quantify hazardous air pollutants
(HAPs) emitted from lime kilns. ESD requested that EPA's Emissions, Monitoring and Analysis
Division (EMAD) conduct the required testing. EMAD issued a work assignment to Pacific
Environmental Services, Inc. (PES) to conduct "screening" tests to collect air emissions data as
specified in the ESD test request. The planning and initial preparation activities of the program
were conducted through EPA Contract No. 68-D7-0002, Work Assignment No. 0/005.
Remaining preparation, testing, and generation of the Draft Final Report were completed under
EPA Contract No. 68-D7-0002, Work Assignment No. 1/007. Generation of the Final Report,
incorporating EPA's comments on the Draft Final Report, was completed under EPA Contract
No. 68-D-98-004, Work Assignment No. 3-03.
The primary objective was to characterize HAP emissions from Lime Kiln No. 1 at the
Chemical Lime Company's facility located in Alabaster, Alabama. The "screening" tests were
conducted to quantify the uncontrolled and controlled air emissions of hydrogen chloride (HC1),
total hydrocarbons (THC), and polychlorinated dibenzo-/?-dioxins and polychlorinated
dibenzofurans (PCDDs/PCDFs). The basic test methods employed were US EPA Test Methods
1 (sample point location), 2 (velocity and volumetric flow), 3A (oxygen and carbon dioxide
concentration), 4 (moisture content), 23 (PCDDs/PCDFs), 25A (total hydrocarbon
concentration), and 26A (hydrogen chloride). Simultaneous testing was performed at the inlet to
the scrubber and at the scrubber stack. Additional analyses of the HC1 train reagents were
conducted to quantify the content of ammonia (NH4), and aluminum, calcium, magnesium,
potassium, and sodium cations. Cybelle M. Brockman of Research Triangle Institute (RTI),
Durham, North Carolina recorded plant operational data during testing. This work was
conducted under a separate work assignment issued to RTI by EPA ESD.
PES used four subcontractors for this effort: Air Pollution Characterization and Control
Inc. (APCC), of Toland, Connecticut; Triangle Laboratories, Inc. (TLI), of Durham, North
Carolina; RTI, and Atlantic Technical Services, Inc. (ATS), of Chapel Hill, North Carolina.
APCC was tasked to provide equipment and manpower for quantification of HC1, O2, CO2, and
total hydrocarbons using continuous emission monitors (CEMs), however no CEMs data was
collected during the field testing effort due to a process upset which occurred the night before
testing was to commence. During the process upset, scrubber liquor flooded the CEM probe,
conditioning system, and the gas filter correlation infrared detector (GCFID) used for HC1
measurements. For this reason, PES used EPA Method 26A for HC1 quantification instead of the
Draft Method 322 as proposed in the Site Specific Test Plan (SSTP). TLI provided analytical
services for the analysis of the PCDDs/PCDFs; RTI provided analytical services for the analysis of
the HC1, NH4, and additional cations, and ATS provided technical support for preparation of the
1-1
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Quality Assurance Project Plan (QAPP), Site Specific Test Plan (SSTP), for reduction of the test
data, and for preparation of the Draft Final Report.
The field testing program organization and major lines of communication are presented in
Figure 1.1. The PES Project Manager (PM) communicated directly with the EPA Work
Assignment Manager (WAM) and coordinated all of the on-site testing activities.
1-2
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Cterncal Lime Company
Environmental, Health & Safety Manager
David R. Christiansen
(817)732-8164
EPA/EMC
Work Assignment Manager
Michael LToney
(919)541-5247
EPA/ESD
Lead Engineer
Joseph P. Wood
(919)541-5466
PES
/ohnT.Chehaske
(919)941-0333
PES
Corporate QA/QC Officer
JefferyL. VanAtten
(703)471-8383
BSD Contractor
CybeBeKBrochmn
(919)990-8654
PES
Project Manager
Franklin Meadows
(919)941-0333
Pretest Ste Survey
PES
SSTP
PES
Subcontractor
QAPP
PES
Subcontractor
Field Testing
PES
Atlantic Technical Sevices, Inc.
Atlantic Technical Services, Inc.
_L
Analysis
PES
Subcontractor
Air Pollution
Characterization & Control, Ltd
Subcontractor
Triangle Laboratories, me.
Report Preparation
PES
Subcontractor
Subcontractor
Atlantic Technical Serivces, Inc.
Figure 1.1 Key Personnel and Responsibility for Testing at Chemical Lime Company - Alabaster, Alabama
1-3
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2.0 SUMMARY OF RESULTS
This section provides summaries of the test results for testing at the Chemical Lime
Company in Alabaster, Alabama. Included are results of the tests conducted for PCDDs/PCDFs,
hydrogen chloride (HC1), ammonia, and additional cation emissions at the Kiln No. 1 Scrubber
Inlet and Kiln No. 1 Scrubber Stack.
2.1 EMISSIONS TEST LOG
PCDDs/PCDFs testing was conducted on Kiln No. 1 on the first day, with the HC1 and
cation testing performed on the second day. Sampling was performed on March 26 and 27, 1998.
Table 2.1 gives the emissions test log. Presented are the run numbers, test dates, pollutants, run
times, and down times for port changes.
TABLE 2.1
EMISSIONS TEST LOG
CHEMICAL LIME COMPANY - ALABASTER, ALABAMA
Run No.
Date
Pollutant
Run Time
Downtime,
Minutes
Kiln No. 1 Scrubber Inlet
M23-I-3
I-M26A-1
I-M26A-2
I-M26A-3
03/26/98
03/27/98
03/27/98
03/27/98
PCDDs/PCDFs
HC1
HC1, NH4, Cations
HC1
1300-1621
0907-1016
1140-1255
1422-1536
23
9
15
14
Kiln No. 1 Scrubber Stack
M23-O-3
O-M26A-1
O-M26A-2
O-M26A-3
03/26/98
03/27/98
03/27/98
03/27/98
PCDDs/PCDFs
HC1
HC1, NH4, Cations
HC1
1300-1632
0909-1028
1140-1255
1423-1538
32
19
15
15
2-1
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2.2 PCDDs/PCDFs
PES employed EPA Method 23 for the measurement of PCDDs and PCDFs. The results
of the PCDD/PCDF results are presented in Tables 2.2 through 2.4. PCDDs/PCDFs results are
presented as 1) actual concentrations and mass emission rates, 2) concentrations adjusted to 7
percent (%) O2, and 3) concentrations adjusted to 7 % O2 and 2378 tetra-chlorinated dibenzo-p-
dioxin (TCDD) toxic equivalent basis. Due to the process upset described previously, no CEM
data was available for the quantification of O2 content in the kiln exhaust streams. Therefore, an
O2 value of 10% was used. This value is typical of the oxygen concentrations observed at other
lime kilns of similar design. Adjustment of the congeners to a 2378 toxic equivalent basis was
calculated using the Toxic Equivalency Factor (TEF) values developed by the NATO Committee
on the Challenges of Modern Society, August 1988.
The Method 23 sample fractions consisted of a sample train front-half solvent rinse, a
paniculate filter, a back-half solvent rinse, and an XAD®-2 sorbent resin module. During analysis,
each of the sample fractions was extracted, concentrated, combined, and analyzed using a Gas
Chromatograph with a Mass Spectrometer detector (GC/MS), according to the procedures
outlined in Method 23. During analysis, the combined sample extract was separated with a DB-5
capillary column. Where the results of that analysis indicated the presence of 2378 TCDF
congeners, the analysis was repeated using a DB-225 capillary column so that the TCDF
congeners could be more readily separated and quantified.
The results of the analyses indicated the presence of several congeners that were qualified
as Estimated Maximum Possible Concentrations, or EMPCs. From time to time during the
Method 23 analyses, a peak elutes at the position expected for a particular congener, but the peak
fails validation based on the theoretical split of chlorine isotopes. That is to say that the number
of Cl35 isotopes and the number of Cl37 isotopes attached to the PCDDs/PCDFs congeners should
agree with the C135/C137 ratio found in nature. For each congener, this ratio must agree within
15%. If the mass ratio of chlorine isotopes does not agree with the natural chlorine isotope ratio,
then the peak is flagged as an EMPC.
The values presented as "Total PCDDs" are the sum of the "12346789 OCDD"
polychlorinated dibenzo-p-dioxin and all of the dioxins labeled "Total"; "Total PCDFs" values are
the sum of the "12346789 OCDF" polychlorinated dibenzofuran and all of the furans labeled
"Total". "Total PCDDs + Total PCDFs" values are the sum of the "Total PCDDs" and "Total
PCDFs" values. Values that have been qualified as being EMPC have been included in the sums.
Concentrations and emission rates based on or including EMPC values are denoted by braces
The isokinetic sampling ratio calculated for Run M23-I-3 was 1 13%, which is outside the
EPA criterion of 90 to 1 10%. The effect of the anisokinetic sampling on the PCDDs/PCDFs
sample is that the particle size distribution in the collected sample may be biased low for large
particles (i.e., particles with diameters greater than about 5 p,m) for the amount of stack gas
sampled. This in turn would tend to bias the detected quantities of the PCDDs/PCDFs congeners
low, if significant quantities of PCDDs/PCDFs are present in the paniculate fraction of the
sample. The worst case (maximum) bias would be approximately 13% if the particle distribution
2-2
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was 100% large particles; a more representative estimate of the low bias would be 7%, based
upon a more probable size distribution of 50% large and 50% small particles.
Due to conflicts with the placement of the CEM probe at the inlet location, Method 23
traverses were not conducted through port D, which may contribute to a low quantification of the
PCDDs/PCDFs, since the velocity pressures observed at port D during the preliminary velocity
traverses were higher than the rest of the duct.
2.3 HYDROGEN CHLORIDE, AMMONIA, AND CATIONS
The HC1, ammonia, and cations emissions sampling and air stream parameters at the Kiln
No. 1 scrubber inlet are summarized in Table 2.5. Table 2.6 presents the HC1, ammonia, and
cations air stream concentrations and emission rates. HC1 and cations emissions sampling and air
stream parameters for the Scrubber Stack are tabulated in Table 2.7, with the HC1, ammonia, and
cations air stream concentrations and emissions presented in Table 2.8.
2-3
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TABLE 2.2
PCDDs/PCDFs SAMPLING AND EXHAUST GAS PARAMETERS
KILN NO. 1 SCRUBBER INLET AND STACK
CHEMICAL LIME COMPANY - ALABASTER, ALABAMA
Run No.
Date
Sampling Location
Total Sampling Time, minutes
Average Sampling Rate, dscfin '
Sample Volume:
dscfb
dscmc
Average Exhaust Gas Temperature, °F
O2 Concentration, % by Volume d
CO2 Concentration, % by Volume d
Moisture, % by Volume
As Measured
At Saturation
Exhaust Gas Volumetric Flow Rate:
acfme
dscfin •
dscmm f
Isokinetic Sampling Ratio, %
M23-I-3
03/26/98
Inlet
180
0.484
87.202
2.469
775
10.0
20.0
14.7
NA
88,500
31,400
889
113.1
M23-O-3
03/26/98
Stack
187.8
0.669
125.554
3.555
137
10.0
20.0
21.1
18.6
42,800
30,300
858
102.7
' Dry standard cubic feet per minute at 68 °F (20 °C) and 1 atm.
b Dry standard cubic feet at 68 °F (20 °C) and 1 atm.
c Dry standard cubic meters at 68°F (20°C) and 1 atm.
d In-stack oxygen and carbon dioxide concentrations assumed due to CEM malfunction.
' Actual cubic feet per minute at exhaust gas conditions.
f Dry standard cubic meters per minute at 68 °F (20 °C) and 1 atm.
2-4
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TABLE 2.3
PCDDs/PCDFs CONCENTRATIONS AND EMISSION RATES
KILN NO. 1 SCRUBBER INLET AND STACK
CHEMICAL LIME COMPANY - ALABASTER, ALABAMA
CONGENER
DIOXINS:
2378 TCDD
Total TCDD
12378 PeCDD
Total PeCDD
123478 HxCDD
123678 HxCDD
123789 HxCDD
Total HxCDD
1234678 HpCDD
Total HpCDD
12346789 OCDD
Total PCDDs
FURANS:
2378 TCDF
Total TCDF
12378 PeCDF
23478 PeCDF
Total PeCDF
123478 HxCDF
123678 HxCDF
234678 HxCDF
123789 HxCDF
Total HxCDF
1234678 HpCDF
1234789 HpCDF
Total HpCDF
12346789 OCDF
Total PCDFs
Total PCDDs + PCDFs
CONCENTRATION •
(ng/dscm, as measured)
M23-I-3 Inlet
(0.00121)
0.00405
(0.00162)
(0.00162)
(0.00283)
(0.00283)
(0.00283)
(0.00283)
(0.00405)
(0.00405)
{0.0121}
(0.0247)
{0.00283}
0.0445
(0.00121)
(0.00121)
0.00810
{0.00283}
{0.0162}
(0.00162)
(0.00202)
0.00405
0.00364
(0.00324)
0.00364
(0.00810)
(0.0684)
(0.0931)
M23-O-3 Stack
(0.00169)
(0.00169)
(0.00253)
(0.00253)
(0.00281)
(0.00281)
(0.00253)
(0.00281)
(0.00281)
(0.00281)
(0.00563)
(0.0155)
(0.00197)
{0.00197}
(0.00169)
(0.00169)
(0.00169)
(0.00169)
(0.00169)
(0.00197)
(0.00225)
(0.00197)
(0.00281)
(0.00281)
(0.00281)
(0.00281)
(0.0113)
(0.0267)
EMISSION RATE b
(ttfi
M23-I-3 Inlet
(0.0648)
0.216
(0.0864)
(0.0864)
(0.151)
(0.151)
(0.151)
(0.151)
(0.216)
(0.216)
{0.648}
(1.32)
{0.151}
2.38
(0.0648)
(0.0648)
0.432
{0.151}
{0.864}
(0.0864)
(0.108)
0.216
0.195
(0.173)
0.195
(0.432)
(3.65)
(4.97)
/hr)
M23-O-3 Stack
(0.0869)
(0.0869)
(0.130)
(0.130)
(0.145)
(0.145)
(0.130)
(0.145)
(0.145)
(0.145)
(0.290)
(0.797)
(0.101)
{0.101}
(0.0869)
' (0.0869)
(0.0869)
(0.0869)
(0.0869)
(0.101)
(0.116)
(0.101)
(0.145)
(0.145)
(0.145)
(0.145)
(0.579)
(1.38)
* Nanogram per dry standard cubic meter at 20°°C and 1 atm.
b Micrograms per hour.
() Not Detected. Value shown is the detection limit and is included in totals.
{ } Estimated Maximum Possible Concentration. EMPC values are included in totals.
2-5
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TABLE 2.4
PCDDs/PCDFs CONCENTRATIONS AND 2378-TCDD TOXIC EQUIVALENT
CONCENTRATIONS ADJUSTED TO 7 PERCENT OXYGEN
KILN NO. 1 SCRUBBER INLET AND STACK
CHEMICAL LIME COMPANY - ALABASTER, ALABAMA
CONGENER
DIOXINS:
2378 TCDD
Total TCDD
12378 PeCDD
Total PeCDD
123478 HxCDD
123678 HxCDD
123789 HxCDD
Total HxCDD
1234678 HpCDD
Total HpCDD
12346789 OCDD
Total PCDDs
FURANS:
2378 TCDF
Total TCDF
12378 PeCDF
23478 PeCDF
Total PeCDF
123478 HxCDF
123678 HxCDF
234678 HxCDF
123789 HxCDF
Total HxCDF
1234678 HpCDF
1234789 HpCDF
Total HpCDF
12346789 OCDF
Total PCDFs
Total PCDDs + PCDFs
CONCENTRATION *
(ng/dscm, adjusted to 7 percent OJ
M23-I-3 Inlet
(0.00155)
0.00516
(0.00207)
(0.00207)
(0.00362)
(0.00362)
(0.00362)
(0.00362)
(0.00516)
(0.00516)
{0.0155}
(0.0315)
{0.00362}
0.0568
(0.00155)
(0.00155)
0.0103
{0.00362}
{0.0207}
(0.00207)
(0.00258)
0.00516
0.00465
(0.00413)
0.00465
(0.0103)
(0.0873)
(0.119)
M23-O-3 Stack
(0.00215)
(0.00215)
(0.00323)
(0.00323)
(0.00359)
(0.00359)
(0.00323)
(0.00359)
(0.00359)
(0.00359)
(0.00717)
(0.0197)
(0.00251)
{0.00251}
(0.00215)
(0.00215)
(0.00215)
(0.00215)
(0.00215)
(0.00251)
(0.00287)
(0.00251)
(0.00359)
(0.00359)
(0.00359)
(0.00359)
(0.0143)
(0.0341)
2378-TCDD
Toricity
Factor
1.000
0.500
0.100
0.100
0.100
0.010
0.001
Total PCDDs TEQ
0.100
0.050
0.500
0.100
0.100
0.100
0.100
0.010
0.010
0.001
Total PCDFs TEQ
Total TEQ
2378 TOXIC EQUIVALENCIES
ng/dscm, adjusted to 7 percent Or
M23-I-3 Inlet
(0.00155)
(0.00103)
(0.000362)
(0.000362)
(0.000362)
(0.0000516)
{0.0000155}
(0.00373)
{0.000362}
(0.0000775)
(0.000775)
{0.000362}
{0.00207}
(0.000207)
(0.000258)
0.0000465
(0.0000413)
(0.0000103)
(0.00420)
(0.00794)
M23-O-3 Stack
(0.00215)
(0.00161)
(0.000359)
(0.000359)
(0.000323)
(0.0000359)
(0.00000717)
(0.00485)
(0.000251)
{0.000108}
(0.00108)
(0.000215)
(0.000215)
(0.000251)
(0.000287)
(0.0000359)
(0.0000359)
(0.00000359)
(0.00248)
(0.00733)
" Nanogram per dry standard cubic meter at 20 °C and 1 atm and corrected to 7 percent oxygen.
() Not Detected. Value shown is the detection limit and is included in totals.
{ } Estimated Maximum Possible Concentration. EMPC values are included in totals.
2-6
-------
TABLE 2.5
HCL AND AMMONIA EMISSIONS SAMPLING AND EXHAUST GAS
PARAMETERS
KILN NO. 1 SCRUBBER INLET
CHEMICAL LIME COMPANY - ALABASTER, ALABAMA
Run No.
Date
Total Sampling Time, minutes
Average Sampling Rate, dscfin "
Sample Volume:
dscf"
dscrn0
Average Exhaust Gas Temperature, °F
O2 Concentration, % by Volume d
CO2 Concentration, % by Volume d
Moisture, % by Volume
Exhaust Gas Volumetric Flow Rate:
acfm'
dscfin "
dscmmf
Isokinetic Sampling Ratio, %
I-M26A-1
03/27/98
60
0.539
32.329
0.915
784
10.0
20.0
15.7
82,600
28,800
816
105.9
I-M26A-2
03/27/98
60
0.487
29.201
0.827
781
10.0
20.0
17.5
79,100
27,100
768
108.8
I-M26A-3
03/27/98
60
0.627
37.602
1.065
775
10.0
20.0
15.9
79,100
27,800
786
106.3
Average
0.551
33.044
0.936
780
10.0
20.0
16.4
80,300
27,900
790
107.0
* Dry standard cubic feet per minute at 68 °F (20 °C) and 1 atm.
b Dry standard cubic feet at 68 °F (20 °C) and 1 atm.
c Dry standard cubic meters at 68 °F (20 °C) and 1 atm.
d In-stack oxygen and carbon dioxide concentrations assumed due to CEM malfunction.
' Actual cubic feet per minute at exhaust gas conditions.
f Dry standard cubic meters per minute at 68°F (20°C) and 1 atm.
2-7
-------
TABLE 2.6
HCL, AMMONIA, AND CATIONS
CONCENTRATIONS AND EMISSION RATES
KILN NO. 1 SCRUBBER INLET
CHEMICAL LIME COMPANY - ALABASTER, ALABAMA
Inn No.
Date
Clock Time, 24-hr clock
Chlorides as HC1
ppmvd
ppmvd @ 7% O2
lb/hrc
Chlorides as Cl
ppmvd a
lb/hrc
Ammonia (as NHt)
ppmvd
lb/hr°
Aluminum, Al
ppmvd a
Ib/hr c
Calcium, Ca
ppmvd a
Ib/hr c
Magnesium, Mg
ppmvd a
Ib/hr °
Potassium, K
ppmvd a
Ib/hr c
Sodium, Na
ppmvd
Ib/hr c
I-M26A-1
3/27/98
0907-1016
8.63
11.0
1.41
8.63
1.37
0.626
0.0507
#N/A
#N/A
#N/A
#N/A
#N/A
#N/A
#N/A
#N/A
#N/A
#N/A
I-M26A-2
3/27/98
1140-1255
8.10
10.3
1.25
8.10
1.21
0.919
0.0700
(0.0216)
(0.00246)
0.109
0.0184
0.0360
0.00370
0.00660
0.00109
0.191
0.0185
I-M26A-3
3/27/98
1422-1536
12.71
16.2
2.00
12.71
1.95
0.814
0.0635
#N/A
#N/A
#N/A
#N/A
#N/A
#N/A
#N/A
#N/A
#N/A
#N/A
Average
9.81
12.5
1.55
9.81
1.51
0.786
0.0614
(0.0216)
(0.00246)
0.109
0.0184
0.0360
0.00370
0.00660
0.00109
0.191
0.0185
Parts Per Million by Volume Dry.
b Parts Per Million by Volume Dry, Corrected to 7% Oxygen.
Pounds per hour.
() Not Detected. Values enclosed in parentheses Q.
#N/A Not Analyzed.
2-8
-------
TABLE 2.7
HCL AND AMMONIA EMISSIONS SAMPLING AND EXHAUST GAS
PARAMETERS
KILN NO. 1 SCRUBBER STACK
CHEMICAL LIME COMPANY - ALABASTER, ALABAMA
Run No.
Date
Total Sampling Time, minutes
Average Sampling Rate, dscfin *
Sample Volume:
dscfb
dscrn0
Average Exhaust Gas Temperature, °F
O2 Concentration, % by Volume d
CO2 Concentration, % by Volume d
Moisture, % by Volume
As Measured
At Saturation
Exhaust Gas Volumetric Flow Rate:
acfme
dscfm"
dscmm f
Isokinetic Sampling Ratio, %
O-M26A-1
3/27/98
62.5
0.653
40.839
1.156
137
10.0
20.0
1 #N/A
18.2
40,900
29,200
826
104.5
O-M26A-2
3/27/98
62.5
0.610
38.098
1.079
137
10.0
20.0
20.0
18.4
39,500
28,100
794
101.4
O-M26A-3
3/27/98
62.5
0.615
38.431
1.088
137
10.0
20.0
20.3
18.4
39,600
28,100
797
102.2
Average
0.626
39.123
1.108
137
10.0
20.0
20.2
18.4
40,000
28,500
806
102.7
' Dry standard cubic feet per minute at 68° F (20° C) and 1 atm.
b Dry standard cubic feet at 68° F (20° C) and 1 atm.
c Dry standard cubic meters at 68° F (20° C) and 1 atm.
d In-stack oxygen and carbon dioxide concentrations assumed due to CEM malfunction.
' Actual cubic feet per minute at exhaust gas conditions.
f Dry standard cubic meters per minute at 68° F (20° C) and 1 atm.
#N/A Not analyzed.
2-9
-------
TABLE 2.8
HCL, AMMONIA, AND CATIONS
CONCENTRATIONS AND EMISSION RATES
KILN NO. 1 SCRUBBER STACK
CHEMICAL LIME COMPANY - ALABASTER, ALABAMA
Run No.
Date
Clock Time, 24-hr clock
Chlorides as HC1
ppmvd a
ppmvd @ 7% O2 b
Ib/hr c
Chlorides as Cl
ppmvd a
Ib/hr c
Ammonia
ppmvd a
Ib/hr c
Aluminum, Al
ppmvd
Ib/hr c
Calcium, Ca
ppmvd a
Ib/hr c
Magnesium, Mg
ppmvd a
Ib/hr c
Potassium, K
ppmvd a
Ib/hr c
Sodium, Na
ppmvd a
Ib/hr c
O-M26A-1
3/27/98
0909-1028
0.968
1.23
0.160
0.968
0.156
0.288
0.0236
#N/A
#N/A
#N/A
#N/A
#N/A
#N/A
#N/A
#N/A
#N/A
#N/A
O-M26A-2
3/27/98
1140-1255
1.33
1.70
0.212
1.33
0.206
0.433
0.0341
(0.0223)
(0.00263)
0.130
0.0227
0.0420
0.00446
0.0450
0.00768
0.115
0.0116
O-M26A-3
3/27/98
1423-1538
1.03
1.31
0.164
1.03
0.160
0.257
0.0203
#N/A
#N/A
#N/A
#N/A
#N/A
#N/A
#N/A
#N/A
#N/A
#N/A
Average
1.11
1.42
0.179
1.11
0.174
0.326
0.0260
(0.0223)
(0.00263)
0.130
0.0227
0.0420
0.00446
0.0450
0.00768
0.115
0.0116
Parts Per Million by Volume Dry.
Pounds per hour.
( ) Not Detected. Values enclosed in parentheses Q-
#N/A Not Analyzed.
2-10
-------
3.0 PROCESS DESCRIPTION
During the testing, an EPA BSD contractor, Research Triangle Institute, monitored and
recorded kiln process operation data. The Chemical Lime Company has made a claim of
confidentially regarding this data, and EPA designated this data as Confidential Business
Information (CBI). Therefore, no process information or operations data has been included with
this report.
3-1
-------
-------
4.0 SAMPLING LOCATIONS
As stated previously, source sampling was conducted to determine uncontrolled and
controlled emissions of HC1, PCDDs/PCDFs, and total hydrocarbons from a lime kiln located at
Chemical Lime Company's Alabaster, Alabama facility. Testing was conducted at the inlet of the
scrubber, and at the stack. Figure 4.1 presents the process air stream schematic showing the
testing locations. Descriptions and schematic diagrams of the test locations are presented below.
4.1 KILN NO. 1 SCRUBBER INLET
The Kiln No. 1 scrubber inlet measurement site was located in a 60-inch by 60-inch
square, vertical duct, 72 inches (1.2 equivalent duct diameters) downstream of the nearest flow
disturbance (90° bend) and 7.5 inches (0.13 equivalent duct diameters) upstream of the fan inlet.
According to EPA Method 1 criteria, this site required 20 sample traverse points. Accordingly,
PES specified a
4x5 sample traverse matrix; four sample points were located on each of five traverses.
Only three ports were accessible. Because of the limited access to port D, the Method 23
and Method 26A sampling was done using three of the four traverse lines. Figure 4.2 shows a
simplified schematic of the inlet measurement site and the sample traverse point locations.
A check for the presence of non-parallel flow was conducted as specified in Section 2.4 of
EPA Method 1. The average yaw angle of 10 degrees was within the Method 1 requirement of a
maximum average yaw angle of 20 degrees.
4.2 KILN NO. 1 SCRUBBER STACK
The scrubber stack measurement site was located in a 58-inch inside diameter (ID) round,
vertical stack, 240 inches (4.1 equivalent duct diameters) downstream of the nearest flow
disturbance (separator exit) and 264 inches (4.6 equivalent duct diameters) upstream of the
nearest flow disturbance, the exhaust to the atmosphere. The Method 23 sampling was performed
using two ports to access the two traverse lines. According to EPA Method 1 criteria, this site
required 24 sample traverse points, 12 along each of two perpendicular diameters. Figure 4.3
shows a simplified schematic of the inlet measurement site and the sample traverse point
locations.
A check for the presence of non-parallel flow was conducted as specified in Section 2.4 of
EPA Method 1. The average yaw angle of 28.8 degrees was greater than the maximum average
4-1
-------
yaw angle of 20 degrees allowed by Method 1. In order to complete this testing, PES employed
an alignment approach whereby the sample nozzle was oriented in the direction of flow as
indicated during the preliminary velocity traverse. The sampling time at each point was calculated
as the product of the base time and the cosine of the yaw angle, a. This approach was used for
both the Method 23 and the Method 26A testing conducted at the scrubber stack.
4-2
-------
Test Location
Test Location
Atmosphere
Stack
Kiln No. 1
Figure 4.1 Kiln No. 1 Process Flow Schematic Showing Testing Locations, Chemical
Lime Company - Alabaster, Alabama
4-3
-------
Traverse Distance from
Point inside wall (in.)
Cross Sectional View
60"
1
2
3
4
5
6
18
30
42
54
60"
0
o
o
0
o
o
o
o
0
o
o
o
o
o
0
o
o
o
o
o
o a LJ cr
A B C D
From Kiln No. 1
Note: Access to
PortD
blocked.
Figure 4.2 Kiln No. 1 Scrubber Inlet Test Location and Traverse Point Locations,
Chemical Lime Company - Alabaster, Alabama
4-4
-------
Cross Sectional View
58"
• • a • • •
• • a o • •
Traverse
Point
Distance from
inside wall (in.)
1
2
3
4
5
6
7
8
9
10
11
12
3 Ve
6 %
10 1/4
14 Vz
20 Ve
37 %
43 1/2
47 a/4
51 1/4
54 V8
56 %
264"
240"
60'
Separator
Figure 4.3 Kiln No. 1 Scrubber Stack Test Location and Traverse Point Locations,
Chemical Lime Company - Alabaster, Alabama
4-5
-------
-------
5.0 SAMPLING AND ANALYTICAL PROCEDURES
Source sampling was performed at the scrubber inlet and the scrubber stack to determine
the concentrations and mass emission rates of HC1, ammonia, aluminum, calcium, magnesium,
potassium, sodium, and PCDDs/PCDFs. Due to greater-than-maximum yaw angles at the
scrubber stack location, the normal isokinetic sampling procedures had to be modified in order to
get the most representative results. The "Alignment Approach" was used to compensate for the
large yaw angles; the Method 23 and the Method 26A trains both used this technique at the stack
location only.
At the scrubber inlet, a 180-minute (three-hour) Method 23 test run and three 60-minute
Method 26A runs were performed. Using the alignment approach, a 187.8 minute Method 23 test
run was performed at the scrubber stack location concurrent with the inlet Method 23 test run.
Three 62.5 minute Method 26A runs were performed at the stack simultaneous with the inlet
Method 26A runs. All three Method 26A runs at each location were analyzed for HC1 and
ammonia, while only the second run was analyzed for aluminum, calcium, magnesium, potassium,
and sodium.
HC1, ammonia, aluminum, calcium, magnesium, potassium, and sodium results are
presented in parts per million (ppm), and pounds per hour (Ib/hr). PCDDs/PCDFs results are
presented in nanograms per dry standard cubic meter (ng/dscm), nanograms per dry standard
cubic meter corrected to 7% oxygen (ng/dscm @ 7% O2) and micrograms per hour (|ig/hr). In
Table 5.1, the parameters measured, the sampling methods, the number of tests performed, and
the duration of each test are given. Brief descriptions of the sampling and analysis procedures
used are presented below.
5.1 LOCATION OF MEASUREMENT SITES AND SAMPLE/VELOCITY
TRAVERSE POINTS
EPA Method 1, "Sample and Velocity Traverses for Stationary Sources," was used to
establish velocity and sample traverse point locations. The process ductwork, and locations of
measurement sites and traverse points are discussed in Section 4.0 of this document.
5-1
-------
TABLE 5.1
SUMMARY OF SAMPLING LOCATIONS, TEST PARAMETERS,
SAMPLING METHODS, AND NUMBER AND DURATION OF TESTS,
CHEMICAL LIME COMPANY, ALABASTER, ALABAMA
Sampling Location
Scrubber Inlet
Scrubber Stack
Parameter
Air Stream Flow Rate
Moisture Content
PCDDs/PCDFs
HC1, Ammonia
Al,Ca,Mg,K,Na
Air Stream Flow Rate
Moisture Content
PCDDs/PCDFs
HC1, Ammonia
Al, Ca, Mg, K, Na
Sampling Methods
EPA Method 2
EPA Method 4
EPA Method 23
EPA Method 26A
EPA Method 26A
EPA Method 2
EPA Method 4
EPA Method 23
EPA Method 26A
EPA Method 26A
Number
of Tests
4
4
1
3
1
4
4
1
3
1
Duration,
M23/M26A
( minutest
180/60
180/60
180
60
60
187.8/62.5
187.8/62.5
187.8
62.5
62.5
NOTE: All tests at the scrubbber stack used the "Alignment Approach" sampling technique for
measurement of stack gas velocity.
5.2 DETERMINATION OF AIR STREAM VOLUMETRIC FLOW RATE
EPA Method 2, "Determination of Stack Gas Velocity and Volumetric Flow Rate (Type S
Pitot Tube)," in conjunction with the "Alignment Approach," was used to determine exhaust gas
velocity. A Type S Pitot tube, constructed according to Method 2 criteria and having an assigned
coefficient of 0.84, was connected to an inclined-vertical manometer and used to measure the
velocity pressure (Ap) in the direction of flow at each traverse point. The air stream temperature
was also recorded at each traverse point using a Type K thermocouple. The average gas velocity
was calculated from the average products of the square root of the velocity pressure and cosine of
the flow angle, average air stream temperature, air stream molecular weight, and absolute stack
pressure. The volumetric flow rate is the product of velocity and the cross-sectional area of the
duct/stack at the sampling location.
As stated previously in Section 4.0, PES conducted cyclonic flow checks according to the
procedures described hi Section 2.4 of Method 1. When the results of a cyclonic flow check
indicated that the flow pattern in the effluent gas stream was unsuitable for conventional isokinetic
sampling (i.e., a > 20°), PES employed a sampling technique known informally as the "alignment
5-2
-------
approach". For gas streams where the flow is cyclonic, or non-parallel with the stack walls,
conventional isokinetic sampling would produce results that are potentially biased with respect to
the true paniculate matter concentration, since the direction of the probe nozzle would not be
aligned with the direction of flow of the effluent gas. Application of the alignment approach
(which is reprinted in Appendix G of this document) is one method that can be employed to
reduce bias in the measurement of paniculate concentration due to non-parallel flow.
In the alignment approach, standard isokinetic sampling procedures are employed, except
that the sampling time at each sample point is adjusted, and the orientation of the pitobe assembly
is adjusted based upon the results of the cyclonic flow check. Using the cyclonic flow check
results, an arbitrary base time is selected. The sampling time at each sample point is determined
by multiplying the base time by the cosine of the flow angle measured at each sampling point. The
base time was adjusted to so that a total sample time of approximately 180 minutes
(approximately 60 minutes for Method 26A) was achieved.
In order to calculate the isokinetic sampling ratio during the sample run, the velocity
pressure at each sample point, measured at the flow angle of each sample point, was used, since
the isokinetic sampling ratio is the ratio of the air velocity through the nozzle to the velocity of the
air stream flowing past the nozzle. In order to calculate the volumetric flow rate of the effluent
gas through the duct, the axial component (i.e., the component of the velocity vectors parallel to
the stack walls) must be determined. At each sampling point, the axial component of the velocity
is directly proportional to the square root of the velocity pressure multiplied by the cosine of the
flow angle. The axial velocity of the gas stream was calculated from the average of these
products, and the effluent gas volumetric flow was calculated by multiplying the resultant velocity
by the cross-sectional area of the duct.
5.3 DETERMINATION OF AIR STREAM MOISTURE CONTENT
EPA Method 4, "Determination of Moisture Content in Stack Gases," was used to
determine the air stream moisture content. EPA Method 4 was performed in conjunction with
each EPA Method 23 test run. Integrated, multi-point, isokinetic sampling was performed.
Condensed moisture was determined by recording pre-test and post-test weights of the impingers,
reagents, and silica gel.
5.4 DETERMINATION OF PCDDs/PCDFs
EPA Method 23, "Determination of Polychlorinated Dibenzo-p-Dioxins and
Polychlorinated Dibenzofurans from Stationary Sources," was used to collect dioxins and furans
at each location. In addition, the proposed rules amending Method 23 as published in the Federal
Register, Volume 60, No. 104, May 31, 1995 were incorporated. These proposed rules correct
existing errors in the method, eliminate the methylene chloride rinse, and clarify the quality
assurance requirements of the method.
5-3
-------
A multi-point integrated sample was extracted isokinetically from the traverse points
shown in Section 4.0. At each traverse point, sampling was performed for 12 minutes at the
scrubber inlet for a total run time of 180 minutes; at the scrubber stack, the sampling probe was
rotated at each sampling point until the nozzle was pointed in the direction of the flow. Each
traverse point was sampled for an amount of time based upon the cosine of the flow angle and the
base time of 9 minutes, resulting in a net run time of 187.8 minutes.
The EPA Method 23 samples were extracted through a glass nozzle, a heated glass-lined
probe, a precleaned and heated glass fiber filter, a water cooled condenser coil and an adsorbent
trap containing approximately 40 g of XAD*-2 adsorbent resin. The EPA Method 23 sampling
train is shown in Figure 5.1.
TLI prepared the filters and adsorbent traps and performed the following analyses. The
samples were extracted and analyzed according to EPA Method 23 and the above mentioned
proposed rules amendment. The sample components (filter, XAD, and rinses) were Soxhlet
extracted and combined. The sample was then split with half being archived and the other half
analyzed. Analysis was performed on a high resolution GC/MS.
5.5 DETERMINATION OF HYDROGEN CHLORIDE, AMMONIA, AND CATIONS
EPA Method 26 A, "Determination of Hydrogen Chloride Emissions from Stationary
Sources," was used (with the "Alignment Approach" at the scrubber stack) to measure the
chloride and ammonia concentrations in the gas streams at the scrubber inlet and stack locations;
in addition, the impingers content from the second run at each location was analyzed for
aluminum, calcium, potassium, magnesium, and sodium. A sample was extracted isokinetically
from each point at each sampling location through a glass nozzle, probe liner, a Quartz fiber
filter maintained at greater than 250 °F, and a series of impingers. The first and second impingers
were each charged with 100 milliliters of 0.1 N sulfuric acid, the third and fourth impingers were
each charged with 100 milliliters of 0.1 N sodium hydroxide, and the fifth impinger contained a
known mass, approximately 200 grams, of silica gel. A schematic of this train is presented in
Figure 5.2.
Pre- and post-test leak checks were conducted on the Method 26A sampling train to guard
against dilution of the collection sample with ambient air. Prior to testing, the train was leak
checked at a system vacuum of at least fifteen inches of mercury, and after each test, the train was
leaked check at the highest system vacuum observed during the test. The maximum acceptable
leakage rate is 0.02 cfrn, and all leak checks that were performed met this criteria.
After each test, the impinger contents were recovered and placed into labeled polypropylene
sample bottles and transported to the analytical laboratory for aluminum, ammonia, calcium,
chlorides, magnesium, potassium, and sodium content analysis. The impinger solutions were
recovered and analyzed by ion chromatography for the ammonia and chloride, and ICP for the
aluminum, calcium, magnesium, potassium, and sodium. The samples were analyzed by the
Center for Environmental Measurement and Quality Assurance of the RTI located in Research
Triangle Park, North Carolina. In addition to the samples, a blank sample of the 0. IN nitric acid
5-4
-------
Temperalure
Sensor
Condenser
Stack
Wall
Button Hook
Nozzle
Gas
Exit
Temperature
Sensor
InclWd Recirculation
Manometer FumP
Empty 100 ml HPLC Water Empty Silica Gel
inclined
Manometer
Vacuum
Pump
Vacuum
Line
Figure 5.1. Sampling Train Schematic for EPA Method 23.
-------
Torpenkn
Senior
O\
TypeS RWTiiie
Figure 5.2 Sampling Train Schematic for EPA Method 26A.
-------
absorbing solution was collected and analyzed to determine the contribution, if any, to the content
from the absorbing reagent.
5.6 DETERMINATION OF CARBON DIOXIDE, OXYGEN, TOTAL
HYDROCARBONS, AND HYDROGEN CHLORIDE
No data were collected due to the damage that was sustained by the PE MCS 100 analyzer during
a process upset. For calculation purposes, 20% was used for CO2 and 10% was used for O2.
5-7
-------
6.0 QUALITY ASSURANCE/QUALITY CONTROL
PROCEDURES AND RESULTS
This section describes the specific QA/QC procedures employed by PES in performing this
series of tests. The procedures contained in the "Quality Assurance Handbook for Air Pollution
Measurement Systems, Volume III, Stationary Source Specific Methods," EPA/600/R-94/038c,
and in the reference test methods served as the basis for performance for all testing and related
work activities in this project.
6.1 CALIBRATION OF APPARATUS
The preparation and calibration of source sampling equipment is essential in maintaining
data quality. Brief descriptions of the calibration procedures used by PES follow.
6.1.1 Barometers
PES used aneroid barometers which are calibrated against a station pressure value
reported by a nearby National Weather Service Station corrected for elevation.
6.1.2 Temperature Sensors
Bimetallic dial thermometers and Type K thermocouples were calibrated using the
procedure described in Calibration Procedure 2a of EPA/600/R-94/038c. Each temperature
sensor was calibrated over the expected range of use against an ASTM 3C or 3F thermometer.
Table 6.1 summarizes the type of calibrations performed, the acceptable levels of variance, and
the results. Digital thermocouple displays were calibrated using a thermocouple simulator having
arangeofO-2400°F.
6.1.3 Pitot Tubes
Type S pitot tubes constructed to EPA Method 2 specifications were used. Pitot tubes
meeting these specifications are assigned to a baseline coefficient to 0.84 and need not be
calibrated. The dimensional criteria and results for each pitot tube used are summarized in
Table 6.2.
6-1
-------
TABLE 6.1
SUMMARY OF TEMPERATURE SENSOR CALIBRATION DATA
Temp.
Sensor
I.D.
7D
T7D
MB-10
RMB-15
Usage
Stack Gas
Stack Gas
Meter Box
Inlet
Outlet
Meter Box
Inlet
Outlet
Temperature, °R
Reference
500
534
666
800
495
533
665
812
493
536
666
492
536
666
493
534
668
493
534
668
Sensor
501
534
665
801
498
535
666
815
494
536
665
494
537
665
495
534
670
493
535
668
Temperature
Difference
0.20%
0.0%
-0.15%
0.12%
0.60%
0.37%
0.15%
0.37%
0.20%
0.0%
-0.15%
0.40%
0.19%
-0.15%
0.40%
0.0%
0.30%
0.00%
0.19%
0.00%
Tolerances
-------
TABLE 6.2
SUMMARY OF PITOT TUBE DIMENSIONAL DATA
Measurement
06 1
«2
Pi
P2
Y
e
A
Z
w
Dt
A/2D,
Criteria
<10°
<10°
<5°
<5°
-
-
-
< 0.125 in.
< 0.03125 in.
0.1875" < Dt<; 0.375"
1.05Dts As 1.50Dt
Acceptable
Assigned Coefficient
Results
Pitot Tube Identification
7D
3
3
1
1
1
0
0.931
0.016
0.0
0.375
1.24
Yes
0.84
T7D
0
1
1
3
0
1
0.973
0.0
0.017
0.375
1.30
Yes
0.84
6-3
-------
6.1.4 Differential Pressure Gauges
PES used Dwyer inclined/vertical manometers to measure differential pressures. The
differential pressures measurements included velocity pressure, static pressure, and meter orifice
pressure. Manometers were selected with sufficient sensitivity to accurately measure pressures
over the entire range of expected values. Manometers are primary standards and require no
calibration.
6.1.5 Dry Gas Meters and Orifices
The EPA Method 23 and Method 26A dry gas meters and orifices were calibrated in
accordance with Sections 5.3.1 and 5.3.2 of EPA Method 5. This procedure involves direct
comparison of the dry gas meter to a reference dry test meter. The reference dry test meter is
calibrated annually using a wet test meter. Before its initial use in the field, the metering system
was calibrated over the entire range of operation as specified in EPA Method 5. After field use,
the metering system was calibrated at a single intermediate setting based on the previous field tesit.
Acceptable tolerances for the initial and final dry gas meter factors and orifice calibration factors
are ± 0.05 and ± 0.20 from average, respectively. The results for the gas meter and orifice used in
this test program are summarized in Table 6.3.
TABLE 6.3
SUMMARY OF DRY GAS METER AND ORIFICE CALIBRATION DATA
Meter
No.
MB-10
RMB-15
Y
Pre-test
1.021
1.000
Post-test
0.985
1.002
% Diff.
-3.6
0.2
EPA Criteria
±5%
±5%
Orifice Coefficient
Average
1.72
1.56
Range
1.59-1.79
1.56- 1.56
EPA Criteria
1.72 ±0.20
1.56 ±0.20
6.2 ON-SITE MEASUREMENTS
The on-site QA/QC activities include:
6.2.1 Measurement Sites
Prior to sampling, the stack and inlet duct were checked dimensionally to determine
measurement site locations, location of velocity and sample test ports, inside stack/duct
dimensions, and sample traverse point locations. Inside stack/duct dimensions were checked
through both traverse axis to ensure uniformity of the stack/duct inside diameter. The inside
stack/duct dimensions, wall thickness, and sample port depths were measured to the nearest 1/16
inch.
6-4
-------
6.2.2 Velocity Measurements
All velocity measurement apparatus were assembled, leveled, zeroed, and leak-checked
prior to use and at the end of each determination. The static pressure was determined at a single
point near the center of the stack or duct cross-section.
6.2.3 Moisture
The EPA Method 23 and Method 26A sampling trains were used to determine the flue gas
moisture content. During sampling, the exit gas of the last impinger was maintained below 68°F
to ensure complete condensation of flue gas water vapor. The total moisture was determined
gravimetrically using an electronic platform balance with 0.1 gram sensitivity. The XAD®
adsorbent module from the EPA Method 23 sampling train was also weighed and its weight
included in the moisture catch.
6.2.4 Method 23 and Method 26A
Table 6.4 summarizes the EPA Method 23 and Method 26A critical field sampling QA/QC
measurements made and the EPA's acceptability criteria. All pre- and post-test sample train leaks
met the acceptance criteria. The isokinetic sampling rates for all runs except I-M23-3 deviated by
no more than 9% from 100%, thereby meeting the method criteria of 90-110%. Run I-M23-3
had an isokinetic rate 113.1%.
EPA Method 23 field blanks were collected near each of the sampling locations to check
for any sample contamination at the sites. Sample trains were assembled and pre- and post-test
leak checks were conducted. The sample trains were recovered in the same manner as the actual
sample runs. Each field blank train was subjected to a minimum of one leak check in the
laboratory and three to five at the sampling site, depending on the location.
6.3 LABORATORY ANALYSES
6.3.1 EPA Method 23 PCDDs/PCDFs
Prior to the field testing program, TLI prepared PES' XAD®-2 adsorbent traps and
precleaned the glass fiber filters. TLFs laboratory QA/QC program consisted of adding
isotopically labeled standards to each sample at various stages of the project to determine
recovery efficiencies. The following types of standards were used:
Surrogate Standards were spiked in the TLI laboratory on the XAD*'-2 resin prior to the
field sampling program. Recovery efficiencies for these surrogate compounds provided a
measure of the sample collection efficiency and an indication of any analytical matrix
effects.
6-5
-------
TABLE 6.4
SUMMARY OF EPA METHODS 23 & 26A FIELD SAMPLING QA/QC DATA
03/26/98
03/27/98
Site
Kiln 1 Scrubber Inlet
Kiln 1 Scrubber Stack
Kiln 1 Scrubber Inlet
Kiln 1 Scrubber Stack
Run No.
M23-I-3
M23-0-3
I-M26A-1
I-M26A-2
I-M26A-3
O-M26A-1
O-M26A-2
O-M26A-3
Pre-Test
Leak Rate
(acfm)
0.004 @ 17" Hg
0.009 @ 15" Hg
0.004 @ 16" Hg
0.013 @16"Hg
0.012 @ 15" Hg
0.008 @ 15" Hg
0.004 @15"Hg
0.005 @ 16" Hg
Post-Test
Leak Rate
(acfm)
0.002 @ 15" Hg
0.010 @ 15" Hg
0.008 @ 13" Hg
0.009 @ll"Hg
0.004 @ 16" Hg
0.003 @ 15" Hg
0.002 @ 12" Hg
0.004 @ 10" Hg
EPA
Criteria
(acfm)
0.02
0.02
0.02
0.02
0.02
0.02
0.02
0.02
Percent
Isokinetic
113.1
102.7
105.9
108.8
106.3
104.5
101.4
102.2
EPA
Criteria
90-110%
90-110%
90-110%
90-110%
90-110%
90-110%
90-110%
90-110%
6-6
-------
Internal Standards were spiked in the TLI laboratory after the field sampling program and
prior to sample extraction. Recovery efficiencies for these compounds were used in
quantifying the actual PCDDs/PCDFs isomers measured in the samples.
Alternate Standards were spiked in the TLI laboratory after the field sampling program
and prior to sample extraction. Recovery of these compounds indicated the extraction
efficiencies.
Recovery Standards were added in the laboratory after extraction just prior to GC/MS
analysis.
Table 6.5 summarizes the recovery efficiencies for the various standards and the respective
quality control limits. In general, the recovery efficiencies for the XAD* blank, field blank, and
samples were all within the method QC limits. Refer to TLI's case narrative for their discussion
of any quality control anomalies.
6.3.2 EPA Method 26A Hydrogen Chloride, Ammonia, & Cations
Tables 6.6 and 6.7 summarize the QA/QC results from the Method 26A laboratory cation
and anion analyses performed by Research Triangle Institute. The field blank analysis results are
presented in Table 6.8.
6-7
-------
TABLE 6.5
SUMMARY OF EPA METHOD 23 STANDARDS RECOVERY EFFICIENCIES
FULL SCREEN ANALYSIS
Internal Standards
2,3,7,8-TCDF
2,3,7,8-TCDD
1,2,3,7,8-PeCDF
1, 2,3,7, 8-PeCDD
1,2,3,6,7,8-HxCDF
1,2,3,6,7,8-HxCDD
1,2,3,4,6,7,8-HpCDF
1, 2,3,4,6,7, 8-HpCDD
1,2,3,4,6,7,8,9-OCDD
Surroeate Standards
2,3,7,8-TCDD
2,3,4,7,8-PeCDF
1,2, 3,4,7, 8-HxCDF
1,2,3,4,7,8-HxCDD
1,2,3,4,7,8,9-HpCDF
Alternate Standards
1, 2,3,7, 8,9-HxCDF
2,3,4,6,7,8-HxCDF
CONFIRMATION ANALYSIS
Internal Standards
2,3,7,8-TCDF
Percent Recovery
TLI
M23
Blank
65.8
67.9
68.6
99.4
68.1
78.7
83.7
92.5
83.0
87.9
106
108
114
90.1
84.5
81.8
69.2
M23
1-3
76.6
71.7
72.6
80.1
101
93.2
99.8
101
65.6
84.9
94.9
87.6
90.8
68.1
80.1
94.0
79.7
M23
0-3
54.8
49.0
55.4
59.7
63.9
72.6
54.3
65.5
63.1
96.7
102
97.4
96.5
95.2
62.9
65.3
60.0
FB-3
Field
Blank
63.8
63.4
64.2
74.3
84.5
97.8
82.6
99.2
104
93.8
99.6
83.7
90.3
85.4
88.0
87.6
*
RB
1-4
Reagent
Blank
66.0
59.9
62.5
76.1
81.6
97.6
82.8
101
115
83.8
101
82.5
82.5
95.2
87.7
89.1
*
QC Limits
40-130%
40-130%
40-130%
40-130%
40-130%
40-130%
25-130%
25-130%
25-130%
70-140%
70-140%
70-140%
70-140%
70-140%
40-130%
40-130%
40-130%
c Confirmation analysis was not necessary on these samples since no TCDF's were detected in the full screen analysis.
6-8
-------
TABLE 6.6
SUMMARY OF EPA METHOD 26A LABORATORY ANALYSIS
QC DATA, ANION SPIKES, AND DUPLICATES
Sample ID
Recovery Efficiency, %
QA-MED
QA-LOW
QA-MED
EPA-3909 b
NH4 QA-1
NH4 QA-2
EPA-3177b
M26A-I-6-A SPIKE c
M26A-O-6-A SPIKE c
Duplicate Analysis
M26A-O-2-A
M26A-O-2-A DUPLICATE
Percent Difference
M26A-O-1-A
M26A-O-1-A DUPLICATE
Percent Difference
Cl
99.0
99.0
100.0
103.4
naa
naa
naa
100.4
naa
0.043 mg/Ld
0.044 mg/Ld
2.3
naa
naa
naa
NH4
naa
naa
naa
naa
96.9
93.6
91.4
naa
96.6
naa
naa
naa
0.019 mg/L
0.018 mg/L
5.3
a na = not applicable
b Quality assurance samples prepared by the EPA.
c Matrix spikes were performed by the laboratory on samples collected at
another lime kiln facility during the same mobilization.
d Milligrams per liter
6-9
-------
TABLE 6.7
SUMMARY OF EPA METHOD 26A LABORATORY ANALYSIS
QC DATA, CATION SPIKES, AND DUPLICATES
Sample ID
Recovery Efficiency, %
M26A-O-2A SPIKE
Duplicate Analysis*
M26A-O-5-ADUP
M26A-O-5-A
Percent Difference
K+
85.0
<4.8ug
<4.8ug
0.0
Ca+
91.8
277 ug
291 ug
-4.8
Mg+
96.2
32.3 ug
33.1 Mg
-2.4
Na+
96.4
40.4 ug
29.6 ug
36.5
AI+
104
15.1 ug
16.1 ug
-6.2
* Duplicate analyses were performed by the laboratory on samples collected at another
lime kiln facility during the same mobilization.
ug - Micrograms
6-10
-------
TABLE 6.8
SUMMARY OF EPA METHOD 26A ANALYSIS
FIELD BLANK RESULTS
Analyte
ci-
NH/
K+
Ca+
Mg+
Na+
Al+
M26A-FB-1-A Catch
0.22 mg
<0.12mg
< 4.3 ng
63.6 ng
12.5 ng
75.0 ng
<13ng
mg - milligrams
Hg - micrograms
6-11
-------
-------
APPENDIX A
RAW FIELD DATA
-------
Appendix A.2
Raw Field Data
Kiln No. 1 Scrubber Outlet
-------
TRAVERSE POINT LOCATION FOR RECTANGULAR DUCTS
/• i * / / '
Pbnfc ^ri+micaS &->•
Date: 3
Sampling Location:.
Duct Width, inches:.
Inside of Far Wall to Outside
Inside of Near Wall to Outside of Nipple (Nipple Length):.
Duct Length, inches:.
Equivalent Diameter - 2xLxW/(L +W) =
Distance Downstream from Flow Disturbance (Distance B):
"7*2- inches / Equivalent Diameter» A~2. dd
Distance Upstream from Fbw Disturbance (Distance A):
~~l**- inches/Equivalent Diameter = <2//3 dd
Calculated By:
Schematic of
Sampling Location
Traverse
Point
Number
/
T.
3
H
5
Fraction
of
Length
O.I
£>.3>
e.S
0.7
'A
Length
(inches)
^0"
Product of
Columns 2 & 3*
(To nearest 1/8")
fr
je
-3>0
H-Z.
^4
Nipple
Length
(inches)
*Vz.
Traverse Point
Location
(Sum of Col. 4 & 5)
y/?v-z.
22 V^
3V v^
Hi, XL
5« vt
If No Ports, Calculate Distances From Stack Walls For Port Locations
Number
of
Potts
Fraction
of
Width
Width
(inches)
Port Location
Product of Col. 2 & 3*
(To Nearest 1/8")
* All points or ports should be an equal distance from each other (D) and 1/2 of
that distance from the stack walls (D/2), where D = Width / # of points or ports
-------
GAS VELOCITY .CYCLONIC, AND VOLUMETRIC FLOW RATE
Sample Location:
Pbar, in. Hg:
Moist, %:
£~k,~ 3-^yw-
P ^
/^ 21^
Stack Dimension, in. Dia. 1 :
Wet Bulb, °F:
Traverse
Point
Number
i
z
3
^
6
i
^
3
f
5
i
7-
3
*f
4
"> \
1^
Tj
t\
£
Average
Velocity
Head, in.
H2O
,56
•bl{
,M
.2-5
jfl
,§(s
, ^8
,*//
.ti~
, 31
'^1
,50
;^5
, 51
iH°l
.to
tftl
."SO
,o "L-
,^ ^
Stack
Temp., °F
"72.0
~nO
*" 7 ^y?
i^
/ Q$
"HO
7CO
-770
~T?0
TJO
I^J^l
**"'7/* s^^
105
73 /
7(j£>
1°\0
160
^7'^
1^7-
i&J
60 no'"
Cyclonic
Flow Angle,
/6
-z
-\
ft
bo
l^
%
t\
o
n
\2>
^
•g
/3
JZ
-n
n
to
.3
/
sq.rtdp Stack Temp Angle,"
HMo3 I -T^/ I
Directon
of Angle
£C
•Ql
^TL^
Cu^
Ct-^S
C + (0.28 X %t^)
Md - (0.44 X ) + (0.32 X ) + (0.26 X )
Md-
% HO % HO
Ma-Mdx(1
Ma- (
Ma-
100
)x(1-
) + 18 ( )
100 100
°R (°F-t-4eO)
13.6
13.8
Pa
in. Hg
Va - 85.49 x Cp x
Va - 85.49 x (
Va- ft/a
Aa- 2-5", 0 n2
Qa-VaxAaxeOa/m
Qa- x
PsxMs
)x
X60
Q.ftd-Q.x17.e47x —
X17.847X-
*H0
100
-------
ro
Sampling Location
Run Number: T.-.3
Pretest Leak Rate: &&(> Operator: P ^Sica,gl_ Nozzle ID: O/2.S Thermo^
Pbar: 21. S Ps: -V.£ Assumed Bws: _5%fifte/#)6
CO2: O2: Meter Box #:wfclc> Y:
in. Hg.
Probe Length/Type: 2l_
Stack Diameter:
Pitot # : -7 t>
As: 3fe<0o'
Post-Test Leak Rate:4,^2. cfm @/^in. Hg.
Post-Test Leak Check: Pitot: Orsat:
S2.
-------
4,
l
T»
Plant
Sampling Location
Run Number: r-2(oA,-( Data: _3-2.-7-a
L^e
Z43
J&Z
1M
jai
Ji5_
^^
^^.
LJ£_
.14^
^43_
I.TL
l.U
£11
241
^_
o.So
353.T.4
144
jLiz.
6.40
JUk
242
J215
143
i
lO'.OO
O.Lb
1.50
l.so
Z4I
7.
Q.MO
i
S2 /f>:^
O.Sl
I.Ha
^42.
^Z
0,53,
i.ao
1.10
807
^7_
i^
Lb^
U.2
07
Due. T
PC
P.T 0
r foei
ZZLE
^
AVm
S. J//..
-------
Sampling Location INU&T
Run Number: X-2.UA-2. Date: 3-ZT-48
Pretest Uak Rate: .o/3 cftn @ /£ in. Hg.
Pretest Leak Check: Pilot: Orsat:
FIELD DATA SHEET
Sample Type: ftl 2. "& A Operator: £
Pbar: ^.5" Ps: ...- 3.7
O2: A
CO2:
Probe Length/Type: 7 '
Slack Diameter: C.Q"*
Pitot #:
"" As: 3Uoo =
Nozzle ID: a. 275 Thermocouple #: 7 fr
Assumed Bws: 13%Filter *:
Meter Box #: 0\(MD Y: jigJ3i_AH@: t,q*f
Post-Test Leak Rate: f). 0pq cfm @// in. Hg.
Post-Test Uak Check: Pitot: Orsat:
PtMFll
NumbM
Swiping
Time
(min)
CkKkTInw
(24-hour
dock)
Gas Meter
Reading
(Vm)fl3
V«tocrty
InHZO
Orilc* Pr«s«ur* Oifterantial
(AH) in H2O
Desired
Actual
Stack
Temp.
(Ts)
Temperature
°F
Probe
Fitter
Impinger
Temp.
°F
Dry Gas Meier Temp.
Inlet
(Tmir»0F)
Outlet
(Tmout°F)
Pump
Vacuum
f«.Hfl)
y///////////////^^^
li:44
0.
1,44,
l.4b
ir.48
O.lb
802-
2 3 to
14-
Z.S
^•77,
1-56
UU
<= &
3.0
1C
53. 3 1
0, 47
20
~2A
12.'. 06
O.S3
240
_2£.
IT.'.
0,4 1
0.41,
742.
£.43
1&
or
.17 «
12-10
6.30
0,70
75"
17.: 2.3
527.00
0.30
0.30
12,
17
2.S
588,73
2.41
LLL
510.
2A\
JL&
o.4U
1.01
.07
±$
11-
0.57
.33
79
24V
k.S
ti'47
. /7
7/35
t.S
244
_£7_
5^
11'. S5
&AI
5^
s
olll
v
-------
FIELD DATA SHEET
Plank
Sampling Location /^Ii6-f TO
Run Number: X~2b\-b Date: 3-2.7-
Pretest Leak Rate: &.o\2. cfm @ tS> in
Pretest Leak Check: Pttot: i/ Orsat:
Sample Type:
Pbar: ^'.5
C02: 12.
Operator:
Ps: "
"02: 4
Hg.
Probe Length/Type: -\ '-
Stack Diameter: fa>"
Pilot #: -7
As:
" 2.6*
Nozzle ID: Q.3M. Thermocouple #: 7 fc
Assumed Bws: j-g, Filter #:
Meter Box #:fv\tblO Y: t.j>v6 AH@: | ,^ 4
Post-Test Leak Rate: 6.oo*f cfm @ /^ in. Hg.
Post-Test Leak Check: Pttot: Orsat:
Point
Number
Sampling
Time
(mto)
Clock Time
(24-hour
dock)
Gas Meter
Reading
fVm)fl3
Velocity
lnH2O
Orillcfl Pressure Differential
(AH) in H2O
Desired
Actual
Slack
Temp.
(Ts)
Temperature
°F
Prot* Filter
Impinger
Temp.
°F
Dry Gas Meter Temp.
Inlet
(TmJn°F)
Outlet
(Tmout°F)
Pump
Vacuum
f«.Hg)
t>.t>2.
X2B
231
^2.
MiL
(*D8. V V
6.5S
2.28
2..-Z.&
/Ol
99
17.
A/I.
£>.*/
/5-'32
X72-
/oo
5
/f>3
$&L
D" rfte M
TO
«r A*
ro
AVm-
-------
MULTI-METALS SAMPLE RECOVERY DATA
wrc&A-T-i
Plant:
Date:
Sample Box No.:
Job No.: l£0tz - GOT-
Sample Location: |
-to
SampleType:
Sample Recovery Person: V\N(MV
Container Description
Volume, ml
Sealed/Level Marked
1
Filter No.(s)
Acetone Rinse
Nitric Rinse
Nitric Rinse - Imp. 1,2,3, + Back 1/2 Filter
5A
Nitric Rinse - Impinger No. 4
5B
KMNO4/H2O Rinse - Impingers 5 & 6
5C
HCI Rinse - Impingers 5 & 6
Impinger
No.
Contents
Initial
/*
Volume, ml
Initial
Weight, grams
Final
Net
I
6.1 N
ico
6-1
.4
6 .\
ico
6V M
r
Total
Comments:
-------
MULTI-METALS SAMPLE RECOVERY DATA
^
-7_
'lant
: C\ Iton- U«*£
Date:
Sample Box No.
Run No.: ggp r*v?
Job No.:
Sample Location:
Sample Type: gg-
Sample Recovery Person:
Container Description
Volume, ml Sealed/Level Marked
Filter No.(s)
Acetone Rinse
Nitric Rinse
Nitric Rinse - Imp. 1,2,3, + Back 1/2 Filter
5A
Nitric Rinse - Impinger No. 4
5B
KMNO4/H2O Rinse - Impingers 5 & 6
5C
HCI Rinse - Impingers 5 & 6
Impinger
No.
Contents
Initial
Volume, ml
Initial
Weight, grams
Final
Net
6 ' N
O.I
Q.i M
(CO
6.1
-------
MULTI-METALS SAMPLE RECOVERY DATA
Plant:
Run No.:
Date:
Sample Box No.:
Job No.:
Sample Location:
Sample Type:
Sample Recovery Person:
Container Description
Volume, ml Sealed/Level Marked
Filter No.(s)
Acetone Rinse
Nitric Rinse
Nitric Rinse - Imp. 1,2,3. + Back 1/2 Filter
5A
Nitric Rinse - Impinger No. 4
5B
KMNO4/H2O Rinse - Impingers 5 & 6
5C
HCI Rinse - Impingers 5 & 6
Impinger
No.
Contents
Initial
Volume, ml
Initial
Weight, grams
Final
Net
-------
MULTI-METALS SAMPLE RECOVERY DATA
3lant: Gfew-
Run No.:
Date:
'5 l?6
Sample Box No.:
Job No.:
ample Location:
|KJit?r
Sample Type: UC Iffa
Sample Recovery Person:
Container Description
Volume, ml Sealed/Level Marked
Filter No.(s)
Acetone Rinse
Nitric Rinse
Nitric Rinse - Imp. 1 ,2,3, + Back 1/2 Filter
5A
Nitric Rinse - Impinger No. 4
5B
KMNO4/H2O Rinse - Impingers 5 & 6
5C
HCI Rinse - Impingers 5 & 6
Impinger
No.
Contents
Initial
Volume, ml
Initial
Weight, grams
Final
Net
5T.G
6
-2. -7
W\T
0. I
Total
Comments:
-------
MULTI-METALS SAMPLE RECOVERY DATA
lant:
Run No.:
Date:
\%
Sample Box No.:
Job No.:
- ooo,
Sample Location: S^rftu&fet Wer
Sample Type: US J
Sample Recovery Person:
Container Description
Volume, ml Sealed/Level Marked
Filter No.(s)
Acetone Rinse
Nitric Rinse
Nitric Rinse - Imp. 1 ,2,3, + Back 1/2 Filter
5A
Nitric Rinse - Impinger No. 4
5B
KMNO4/H2O Rinse - Impingers 5 & 6
5C HCI Rinse - Impingers 5 & 6
Impinger
No.
Contents
Initial
Volume, ml
Initial
Weight, grams
Final
Net
1M.
ICD
.0
\0o
Q38.4
Total
Comments:
-------
FIELD DATA SHEET
Plant ^uefouiAL LifA£
Sampling Location /Mrr n>
Run Number:
-h
Pretest Leak Rate: t,oo'
Pretest Leak Check: Pitot:
elm @ /j" in. Hg.
Orsat:
Sample Type: (Y[ 23 Operator:
Pbar: 2^.5 Ps: -V. ^ ''
CO2: O2:
Probe Length/Type: £_
Stack Diameter: teo^*±
Nozzle ID: Q.2.S
Assumed Bws:
Meter Box)
Thermocouple #:
Filter #:
Y:
As: 3Ltx>1
H@: i.uf
dock)
Ga
-------
Appendix A.2
Raw Field Data
Kiln No. 1 Scrubber Outlet
-------
TRAVERSE POINT LOCATION FOR CIRCULAR DUCTS
Plant:.
Date:
Sampling Location: ^>c
Inside of Far Wall to Outside of Nipple: la
~ f(lLfJ
Inside of Near Wall to Outside of Nipple (Nipple Length):.
Stack I.D.:
Distance Downstream from Flow Disturbance (Distance B):
' 1HP inches / Stack I.D. = 4«( dd
Op
Distance Upstream from Flow Disturbance (Distance A):
?3-' &H inches / Stack I.D. =
Calculated By:
dd
Schematic of
Sampling Location
Traverse
Point
Number
I
2
3
H
5
L
1
$
t
10
I/
i^
Fraction
of
Length
. 62.1
~l
. 11%
. n~i
ISO
'35C?
>C4
2^,^
zt>,c
vz.y
414
-$"?."?
•S-7,2,
^./
6^
-------
GAS VELOCITY .CYCLONIC, AND VOLUMETRIC FLOW RATE
Plant:
rtkhdJU/ -Crt^mUi^t
Sample Location:
Run No.:
Pbar, in. Hg:
Moist, %:
ir^uL, a^^- k.L
j
in 5,
A i/n ^
a ^q.6
i?>Y»
Stack Dimension, in. Dia. 1 :
Wet Bulb, °F:
Traverse
Point
Number
/
-7
3
1
5
Lr
7
6
°l
10
n
(2-
/
I
?
1
5
V
7
1
"I
10
'I
>L
Velocity
Head, in.
H,0
.k(s
.^3^(5
'"^fc
.53
.S2-
1%
• SS
L?2
.S8
,50
.35
.47
.72
'{/5
•7
1^-7
/37
i?n
/31
/3~7
/^-7
/3~)
'31
'3-?
/il
/S<^
/3sr
5^ "
— -
Cyclonic
Flow Angle,
T--5
2-5
Z-fT
2$
10
i&
3£>
AC?
JO
3^
3-5
15
yo
37
^D
33
i&
23
3D
^0
1?C>
^0
32;
36
sq.rt dp Stack Temp Angle, °
Directon
of Angle
CuJ
C JA ft
Date: ^^ ^f
Clock Time: 15": oo
Operators: ~fa-j£tG>~ )9\/h Mf
Static Pressure, in. H2O: — . -SO v
Pilot Tube, Cp: *W &^ '-**
Dia. 2: ^ "
Dry Bulb, °F:
Md - (0.44x%CX)2) + (0.32 x%O2) + (0.28 x%Nj)
Md - (0.44 X ) + (0.32 X ) -i- (0.28 x )
Md -
% H2O % H2O
Ms - ( )x(1- ) + 18( )
100 100
Ms-
TS- °F- °R(°F + 460)
P, , pb + ..?.-f :. - < ) +
13.8 ' ' 13.8
Ps- 2A.|^ in. Hg
F= J Ts<°R)
Vs-85.4WxCpxVAP x ^ psxM8
V» - fl5,49 x ( )•*( ) X A I ..
V*. ft/a
A.- n2
Q» - Va x As x 60 a/m
Q«. x x80
Qt • ^J I') | ^c acfm
Q« .j-QtX 17.847 x x(1 -^-)
•to T« 100
std 100
Q-ttd- Jl
-------
ALL(rr
5
Plant: C&
HAH ViTi nfiTv AMR v/^i i "i
^ 33
£ )6
c. Z^
7 30
8 3(5
9 30
/o SO
I/ 2>5
'2_ 35
'**- °\^Mc,^ 1 3 >
pOjjSHl
W"^
.s»
• ^1
,0,
.?g
• iy
.^s
• S7
•^
-?7
• S?
• ?2
»«2
,*7T
.«o
.17
.•81
Cko
A <4
•«7
.?7
•0 I
•?1
M
-1Z
f
2°TfS1
^f
9. Z >,J?^7
y.?
?.Z-
1. °\
1.S
$.1
7.8
ff-S
7.^
7.1
•7-Y
-?.*/
U°l
>?_
f,.1
7-C?
?.5?
$.3
7-5
7tf
If5
7«3
T*f
1-^
^p-
^ 2..1
•2-O
2-' C-
2v^
2 ^
2.^
^-^
i.fo
£-5"
a.5"
2.^
^ ^
^v2/
,^
^-3
ex
2.£.
2 ^
2.0
s.r
^^
T.-
M (V
Md - <0.44x%CQ2) » (0.32 x%O2) -r (0.28x%Nj)
Md - (0.44 x ) * (0.32 x ) + (0.28 x )
Md -
% H,O % K,O
100 100
M« mi \ V M . 1 -*- Ifl I _.„ „.,. \
100 100
Ml-
c p
Pfl _ P(-I + J-^ ( ) ^ ... _,.,,
13.0 13.0
P» - in. Hg
VS^ =
[ 7i (°R)
v.-6b.4yxu3x^P x ^ paxM8
Vt - n*i 49 x ( ) > ( ) * A I
Vi - ft/1
A.- n2
Qi - Vi x Ai x 00 l/m
Ql - x X00
Qi - «dm
Pi *H,0
Qi^ .- Ql x 17.647 x x (1 • =— )
•" T« 100
•" 100
-------
GAS VELOCITY .CYCLONIC, AND VOLUMETRIC FLOW RATE
Plant:
CJxtm.^i j^.^ -Q\l«bL.4- £/„
0-#4'l
*A
Pbar, in. Hg: ^ .5
Moist, %:
Stack Dimension, in. Dia. 1 :
Wet Bulb, °F:
\
Traverse
Point
Number
1
I
1)
q
^
u
-7
%
i)
ID
\(
II
i
z
^
*f
5
b
-l
%
f
ID
\l
\ls
Average
Velocity
Head, in.
H2O
^
$
<\
StacV
Temp.^F,
i*
T-C
-2<
•*>
7-0
10
^
Z°
3o
1C
1<
?<-
10
31
1»
21
>o
ii
34
Jo
3o
36
*<•
5<
Cyclonic
Flow 4^g'e>
,Z<3
3--L
-Z~2^
Z-6
>5
/O
15
2-G
20
35-
3g-
3c>
^
^-5
^^i
3d)
IO
} 5
2<;
2.4
25
^O
o,0
"^O
sq.rt dp Stack Temp Angle, °
I
Directon
of Angle
£ou
^VO
^U>>
Ct-U
^^
^.ut^
<£C
{C
<^:
c^
<^<
t<;
cuJ
(L\jJ
/*A_jf_f,S
^ {jLS
|
Vs - 85.48 x ( ) x ( ) x \ I
V8- ft/8
A.. n2
Qs- VsxA8x608/m
Qs- x xOO
Qs • acfrn
p, %H,0
Qt^j- Qt xl 7.847 x x(1- * • )
SKI Jg 100
•
«"e1d- Aif.w.i« » 10Q .
dtctnt
-------
I t>
Plant
Sampling Location
Run Number: f)-
Date:
FIELD DATA SHEET
Sample Type: /K-.23 Operator:
Pbar: Z1.S Ps: - n.
CO2: tz. O2: _ Thermocouple #: if)
Assumed Bws: . /4/ Fitter *:
Meter Box #:K»B/S Y: -3^ AH@: /. %
Pretest Leak Rate: .oo'? elm @ /5" in. Hg.
Pretest Leak Check: Pitot: //Great: —
Probe LengtoVType:
Stack Diameter:
Post-Test Leak Rate: QJO cfm
in. Hg.
As:
Post-Test Leak Check: Pilot: <—-Orsat:
Point
Number
Sampling
Tbm
(tnin)
dock Time
(24-hour
dock)
Gas Meter
Raadino
Velocity
Head (Ap)
inH2O
Orifice Pressure Differential
(AH) in H2O
Desired I Actual
Stack
T«mp.
(Ts)
Temperature
Probe
FOter
Impinger
Temp.
°F
Dry Gaa Meter Temp.
Intel
(Tmin0F)
Outlet
(Tmout°F)
Pump
Vacuum
f«.Hg)
////////////////////////////////////////////////////////////,
*>
(e
10
II
a,
JL
,L«Z-
273.0
^^_
f^-%)
HM.
HI.I
J2ill
-ai
1.1
_LH
^£.
JuL.
z,
0,63
2,0
TT
2
/.S
TB:
I'M.
ZS!
2.6O
2.41
J-SO
*7
1S2-
24 1
5/
SZ.
53
.5":$
50
57
E
AH- J.
1*
±
sr
/^? «
J3L
.
-------
FIELD DATA SHEET
0.AU.-V- X-'U*!
Plant
Sampling Location
Run Number: Q-.&A-V Date: 3-2.7-^
Pretest Leak Rate: .Ooff cfrn @ '5 in. Hg.
Pretest Leak Check: Pitot: tXOrsat: -—-
Sample Type:
Pbar: jtf-5_
C02:
Operator:
/2_
Ps:
O2:
K - 3. 2.M
Nozzle ID: .25(3 Thermocouple #: l£)
Assumed Bws: ig Filter #:
Meter Bon it:,
Y:
Probe Length/Type: l'(,U& Pitot #: ID
Stack Diameter: 5"^* As: 18-3^ •ft1'
Post-Test Leak Rate: ,«9g>:3cfm @/JTin. Hg.
Post-Test Leak Check: Pitot: tXOrsat: — -
t>
Tr
•%- 1 •
rwni
Numbai
O
10
ff
Samplng
Time
(mln)
27.
S2JL
Clock Time
(24-hour
dock)
A
Gas Meter
Reading
(Vm)ft3
375 65 q>
3)12. 3
-MO/.
, ^
Velocity
Hwd(Ap)
InHZO
Oriflca Pressure Difhrential
(AH) n H2O
Desired | Art"«l
Stack
Temp.
(Ts)
Temperature
°F
Probe
Filter
bnpinger
Temp.
°F
Dry Gas Meter Temp.
Inlet
(Tmin0F)
Outlet
(Tm oul°F)
Pump
Vacuum
f«.Hg)
Y////////////W
,53
.37
7.5
-U/
2-3
1.7
1.1
1-2
I.I
I.I
M
'7
U-
l.L
A 5
y.z
1,1
A
fbL*
'36
/36
13.7
/37
^1Z
^2X
265
266
Aki.
7CV
1-70
Z70
2^-7
*Li
11
-7C,
77
77
76*
7?
7?
50
73
•73
r-
7-T
70?
24
^i
is-
T7S-
-7
/o
/a
/o
$>
-17/2.
-------
t-Ui
/O
FIELD DATA SHEET
Plant
Sampling Location
Run Number:
Pretest Leak Rate:
Pretest Leak Check: Pilot: v/ Orsal: - .
Date:
Sample Type:
Pbar: ^.^
CO2: /z
_ Operator:
Norzle ID:
Ps:
02:
Thermocouple It: 7&
FHter #:
Y:
cfrn @ 15 in. Hg.
Probe Lengthflype: 7'
Stack Diameter: 5?"
Pilot #: "7Q
As: /1-35" -f/
Assumed Bws
Meter Box *:
Post-Test Leak Rate: , p^ cftn @^in. Hg.
Post-Test Leak Check: Pilot: ^ Orsat: —~
/
A.
tl3"7
. 3
V. f
575
(.0
^3^3.6
'•»-\ -
. -T
. 3-5"
62.
Ul
. 1
A3
/.s
X8
A3
,(A\\ AH
'37
122.
±£L
?t
j^2
26 /
259
231
g^>
jZo^>
31
XL
a
#5
^L
xo
'0
/a
XO
''O
;o
33/1*1
-------
Sampling Location _
Run Number: o
Date: ?>-
Pretest Leak Rate: -00.5 cftn @ '& in. Hg.
Pretest Leak Check: Pitol: iXOrsat: —
FIELD DATA SHEET
Sample Type: /r\ - Tj^fr Operator:
Pbar: 24.5 Pi:
CO2: ,2. O2:
Probe Length/Type: 7'
Stack Diameter: 5£ "
Thermocouple *: ID
Pitol #:
As:
.ft
Nozzle ID:
Assumed Bws: „ /g1 Filler #:
Meter Box »:.
-------
MULTI-METALS SAMPLE RECOVERY DATA
Plant:
~Ct
*c?
Run No.:
Date:
Sample Box No.:
Job No.:
Sample Location:
Sample Type: .U5
Sample Recovery Person: \AA.
-------
MULTI-METALS SAMPLE RECOVERY DATA
- 0-J.
Plant:
Run No.:
Date:
Sample Box No.:
Job No.:
Sample Location:
Sample Type: U
Z&fr
Sample Recovery Person: \A/\lO\W
Container Description
Volume, ml
Sealed/Level Marked
Filter No.(s)
Acetone Rinse
Nitric Rinse
Nitric Rinse - Imp. 1 ,2,3, + Back 1/2 Filter
5A
Nitric Rinse - Impinger No. 4
5B
KMNO4/H2O Rinse - Impingers 5 & 6
5C
HCI Rinse - Impingers 5 & 6
Impinger
No.
Contents
Initial
Volume, ml
Initial
Weight, grams
Final
Net
o
V4
100
C.\H
Total
Comments:
-------
MULTI-METALS SAMPLE RECOVERY DATA
'lant:
RunNo.:
Date:
Sample Box No.:
Job No.: fad. -
Sample Location:
Sample Type:
1C*
Sample Recovery Person:
Container Description
Volume, ml Sealed/Level Marked
Filter No.(s)
Acetone Rinse
Nitric Rinse
mes.'ofi:s3!s
Nitric Rinse - Imp. 1,2,3, + Back 1/2 Filter
5A
Nitric Rinse - impinger No. 4
5B
KMNO4/H2O Rinse - Impingers 5&Q
5C HCI Rinse - Impingers 5 & 6
Impinger
No.
Contents
Initial
Volume, ml
Initial
Weight, grams
Final
Net
-G
Kl
(,40.0
Total
Comments:
-------
MULTI-METALS SAMPLE RECOVERY DATA
Plant: ( >feyiA U*^
Sample Location: :x/M
SampleType: (/T
Sample Recovery Person:
Container Description
Volume, ml
Sealed/Level Marked
Filter No.(s)
Acetone Rinse
Nitric Rinse
Nitric Rinse - Imp. 1,2,3, + Back 1/2 Filter
5A
Nitric Rinse - Impinger No. 4
5B
KMNQ4/H2O Rinse - Impingers 5 & 6
5C IHCI Rinse - Impingers 5 & 6
Impinger
No.
Contents
Initial
Volume, ml
Initial
Weight, grams
Final
Net
O.l A'
./ M
p.l M
632,8
Total
Comments:
-------
MULTI-METALS SAMPLE RECOVERY DATA
\tfiHT
Plant
Run No.: j/UTM-Pfe-J-
Date: 3
Sample Box No.:
Job No.: ftat -
Sample Location:
&x
n~ef
Sample Type:
US
Sample Recovery Person:
Container Description
Volume, ml Sealed/Level Marked
Filter No.(s)
Acetone Rinse
Nitric Rinse
Nitric Rinse - Imp. 1 ,2,3, + Back 1/2 Filter
5A
Nitric Rinse - Impinger No. 4
5B
KMNO4/H2O Rinse - Impingers 5 & 6
5C
HCI Rinse - Impingers 5 & 6
Impinger
No.
Contents
Initial
Volume, ml
Initial
Weight, grams
Final
Net
\
6- 1 Kl
loo
lew
£>.[
ICO vuJL
£> - 1 Kl
Total
Comments:
-------
-------
APPENDIX B
LABORATORY ANALYTICAL DATA
-------
Appendix B.I
Laboratory Analytical Data
Method 26A
-------
TECHNICAL REPORT
Client: Pacific Environmental Services
Purchase Order No.: 104-98-0175
RTI Project No.: 91C-7048-03E
Date: April 21,1998
By
Eva D. Hardison
Research Triangle Institute
Post Office Box 12194
3040 Comwallis Road
Research Triangle Park, NC 27709
(919) 541-5926
Submitted to:
Frank Phoenix
Pacific Environmental Services
5001 South Miami Blvd., Suite 300
Research Triangle Park, NC 27709
/RTI
-------
INTRODUCTION
Seven impinger samples were received under Purchase Order No. 104-98-0175 on April
9,1998 for analysis of chloride and ammonium ions.
ANALYSIS
The samples were analyzed on a Dionex Model DX-500 Ion Chromatograph using
conductivity detection and data reduction by Dionex PeakNet software. Chloride ion
was analyzed using a Dionex AS12A anion separator column and ammonium ion was
analyzed using a Dionex CS12 cation separator column. Quality control samples
prepared by RTI and quality assurance samples prepared by the Environmental
Protection Agency (EPA) were used to verify the calibrations. A sample matrix spike
and a duplicate were also analyzed.
RESULTS
See spreadsheets.
COMMENTS
No problems were encountered.
SAMPLE CUSTODY
Samples will be kept for 3 months after the report is delivered.
Page 1 of 1
/RTI
-------
Analysis of Impinger Absorbing Solutions for Cl and NH4
Pacific Environmental Services
Sample Receipt Date: 4/9/98
Sample Analysis Date: 4/15/98; 4/20/98
PES P.O.* 104-98-0175
RTI Project No. 91C-7048-03E
Sample ID
M26A-I-1-A
M26A-I-2-A
M26A-I-3-A
M26A-O-1-A
M26A-O-2-A
M26A-O-3-A
M26A-FB-1-A
Cl, ug/mL
0.321
0.266
0.522
0.032
0.043
0.042
0.009
•in i*i"* ^^^i1 1 • " |
45
DF Vol.mL Cl, mg I
100
100
100
100
100
100
100
363
371
382
516
493
392
241
11.65 //.9?
9.87 1 0.1?
19.94 2.0, S\
1.65 1.^0
2.12 *.!#
1.65 I >~10
0.22
Report Date: 4/20/98
NH4, ug/mL
0.047
0.061
0.068
0.019
0.028
0.021
<0.020
DF Vol. mL NH4, mg
25
25
25
25
25
25
25
363
371
382
516
493
392
241
0.43
0.57
0.65
0.25
0.35
0.21
<0.12
-------
QA/QC for
Analysis of Impinger Absorbing Solutions for Cl and NH4
Pacific Environmental Services
Sample Receipt Date: 4/9/98
Sample Analysis Date: 4/15/98; 4/20/98
Report Date: 4/20/98
Cl, exp.
Sample ID mg/L
QA/QC:
QA-MED 0.500
QA-LOW 0.200
QA-MED 0.495
EPA-3909 0.502
NH4 QA-1 NA
NH4 QA-2 NA
EPA-3177 NA
Spikes:
M26-I-6-A 1/100 OIL
Spike 0.553
M26A-O-6-A 1/25 OIL
Spike
Duplicates:
M26A-O-2-A 1/100 OIL
M26A-O-2-A DUP 1/100 OIL
M26A-O-1-A 1/25 OIL
M26A-O-1-ADUP 1/25 D!L
Cl, found
mg/L % Rec.
0.495 99.0
0.198 99.0
0.495 100.0
0.519 103.4
NA
NA
NA
0.153
0.555 100.4
0.043
0.044
NH4, exp. NH4, found
mg/L mg/L
NA NA
NA NA
NA NA
NA NA
5.000 4.844
0.500 0.468
0.444 0.406
1.514
2.514 2.428
0.019
0.018
% Rec.
96.9
93.6
91.4
96.6
-------
TECHNICAL REPORT
Client: Pacific Enviromnental Services, Inc.
Purchase Order No.: 104-98-0175
RTI Project No.: 7048-03E
Date: April 23,1998
By
KateK.Luk
Research Triangle Institute
Post Office Box 12194
3040 Comwallis Road
Research Triangle Park, NC 27709
(919)541-6569
Submitted to:
Frank Phoenix
Pacific Environmental services, Inc.
5001 South Miami Blvd., Suite 300
RTF, NC 27709-2077
/RTI
-------
RTI Project No.: 7048-03E
Samples: Impinger Samples
Company: PES (P.O.# 104-98-0175)
Analyte: Trace metals
Method of Analysis: ICP
Sample Received Date: 4-9-98
Analysis Date: 4-16-98
Report Date: 4-23-98
Table 1. Results for Impinger Samples
Sample
M26A-I-2-A
M26A-O-2-A
M26A-FB-1-A(inlet)
M26A-I-5-A
M26A-O-5-A
M26A-FB-2-A(inlet)
Total
Volume
ml_
371
493
241
227
269
197
K
ug
8.87
78.9
<4.3
9.51
<4.8
<3.5
Ca
ug
150
233
63.6
145
291
80.8
Mg
ug
30.1
45.8
12.5
18.6
33.1
10.2
Na
ug
151
119
75.0
47.9
29.6
27.0
Al
ug
<20
<27
<13
<12
16.1
<11
Detection Limit: K - 0.018 ug/mL
Ca - 0.003 ug/mL
Mg - 0.001 ug/mL
Na- 0.065 ug/mL
Al - 0.054 ug/mL
Page 2 of 3
-------
RTI Project No.: 7048-03G
Samples: QC for Impinger Samples
Company: PES (P.O.# 104-98-0175)
Analyte: Trace metals
Method of Analysis: ICP
Sample Received Date: 4-9-98
Analysis Date: 4-16-98
Report Date: 4-23-98
Sample
QC
QC Epected
QC
QC Expected
Table 2. Calibration Check Sample
K Ca Mg Na Al
ug/mL ug/mL ug/mL ug/mL ug/mL
Measured Measured Measured Measured Measured
0.0432
0.0500
0.0497
0.0500
2.05
2.00
1.01
1.00
2.06
2.00
10.0
10.0
2.10
2.00
5.12
5.00
10.1
10.0
20.1
20.0
Sample
RTI-Blk
M26-O-2A SPK
SPK Expected
% SPK Recovery
Table 3. Results of Blank and Spike Analysis
K, ug/mL
Measured
< 0.018
0.340
0.400
85.0
Ca, ug/mL
Measured
< 0.003
0.459
0.500
91.8
Mg, ug/mL
Measured
< 0.001
4.81
5.00
96.2
Na, ug/mL
Measured
< 0.065
2.41
2.50
96.4
Al, ug/mL
Measured
< 0.054
5.22
5.00
104
Sample
Table 4. Results of Duplicate Analysis
K, ug Ca, ug Mg, ug Na, ug Al, ug
Measured Measured Measured Measured Measured
M26-O-5-A DUP
<4.8
277
32.3
40.4
15.1
Page 3 of 3
-------
Appendix B.2
Laboratory Analytical Data
Method 23
-------
CASE NARRATIVE
Analysis of Samples for the Presence of
Polychlorinated Dibenzo-p-Dioxins and Dibenzofurans by
High-Resolution Chromatography / High-Resolution Mass Spectrometry
Method 23 (6/93)
Date:
Client ID:
P.O. Number:
TLI Project Number:
April 21,1998
Pacific Environmental Services
104-98-0159
45399
This report should only be reproduced in full. Any partial reproduction of this report requires permission from
Triangle Laboratories, Inc.
Rev. 11/19/97
Triangle Laboratories, Inc.
801 Cap/to/a Drive P.O. Box 13485
Durham, NC 27713-4411 Research Triangle Park, NC 27709-3485
919-544-5729 Fax #919-544-5491
Off!
-------
Triangle Laboratories, Inc. April 21,1998
Case Narrative 45399
Overview
The sample(s) and associated QC samples were extracted and analyzed according to
procedures described in Method 23 (6/93). Any particular difficulties encountered during
the sample handling by Triangle Laboratories will be discussed in the QC Remarks section
below. This report contains results only from the Method 23 dioxin/furan analyses of the
M23 sample(s).
Quality Control Samples
A laboratory method blank, identified as the TLIM23 Blank, was prepared along with the
samples.
Quality Control Remarks
This release of this particular set of Pacific Environmental Services analytical data by
Triangle Laboratories was authorized by the Quality Control Chemist who has reviewed
each sample data package following a series of inspections/reviews. When applicable,
general deviations from acceptable QC requirements are identified below and comments
are made on the effect of these deviations upon the validity and reliability of the results.
Specific QC issues associated with this particular project are:
Sample receipt: Twelve M23 sample(s) were received from Pacific Environmental
Services in good condition on April 01,1998 at ambient temperature and stored in a
refrigerator at 4 °C. On the sample labeled M23-0-1-2, acetone was marked through and
toluene was written above it. On the sample labeled M23-0-1-3, toluene was marked
through and acetone was written above it. Neither of these labels agreed with the clients'
chain of custody.
Sample Preparation Laboratory: None
Mass Spectrometry: None
Data Review: Sample M23-O-1 indicated low internal standard recoveries. However, the
signal-to-noise ratio is above ten-to-one in all cases and all standards are valid for
quantitation. TCDF was the only analyte detected in this sample and is below Target
Detection Limit (TDL).
-------
Triangle Laboratories, Inc. April 21,1998
Case Narrative 45399
Other Comments: No 2,3,7,8-substituted target analytes were detected in the TLI Blank
above the target detection limit (TDL).
The analytical data presented in this report are consistent with the guidelines of EPA
Method 23 (6/93). Any exceptions have been discussed in the QC Remarks section of
this case narrative with emphasis on their effect on the data. Should Pacific
Environmental Services have any questions or comments regarding this data package,
please feel free to contact our Project Scientist, Rose West, at 919/544-5729 ext. 270.
For Triangle Laboratories, Inc.,
Released by
Girgis Mikhael
Report Preparation Chemist
The total number of pages in the data package
-------
TRIANGLE LABORATORIES, INC.
LIST OF CERTIFICATIONS AND ACCREDITATIONS
ENVIRONMENTAL
American Association for Laboratory Accreditation. Accredidation pending. Certificate
Number 0226-01. Accreditation for technical competence in Environmental Testing.(Including
Waste Water, Sol/Haz Waste,. Pulp/Paper, and Air Matrices) Parameters are AOX/TOX, and
Dioxin/Furan. Method 1613 for Drinking Water.
State of Alabama, Department of Environmental Management Expires December 31. 19S8.
Laboratory I.D. # 40950. Dioxin in drinking water.
State of Alaska, Department of Environmental Conservation. Expires December 21. 19S8.
Certificate number OS-OQ397. Dioxin in drinking water.
State of Arizona, Department of Health Services. Expires May 26. 1998. Certificate 3AZQ423.
Drinking Water for Dioxin, Dioxin in WW and S/H Waste.
State of Arkansas, Department of Pollution Control and Ecology. Expires February 18, 1999.
Pulp/paper, soil, water, and Hazardous Waste for Dioxin/Furan; AOX/TOX, Volatiles, Semi-
volatiles, and Metals.
State of California, Department of Health Services. Expires August 31, 1999. Certificate
#1922. Selected Metals in Waste Water, Volatiles, Semi-volatiles, and Dioxin/furan in WW and
Sol/Haz Waste. Dioxin in drinking water.
State of Connecticut, Department of Health Services. Expires September 30, 1999.
Registration #PH-0117. Dioxin in drinking water. . ..
Delaware Health and Social Services. Expires December 31,1998. Certificate #NC 140. Dioxin
in drinking water.
Florida Department of Health and Rehabilitative Services. Expires June 30, 1998. Dioxin in
DW. Drinking Water ID HRS# 87424. Metals, Extractable Organics (GC/MS), Pesticides/PCB's
(GC) and Volatiles (GC/MS) in Environmental Samples. Environmental water ID HRS# E87411.
RmiMd 3O/98 RM
yicertifidcertiistmem
-------
Hawaii Department of Health. Expires March 1, 1999. Dioxin in drinking water. "Accepted"
status for regulatory purposes.
Idaho Department of Health and Welfare. Expires December 31, 1998. Dioxin in drinking
water.
State of Kansas, Department of Health and Environment Expires January 31, 1999.
Environmental Analyses/Non portable Water and Solid and Hazardous Waste. Method 1613 for
drinking water. ID #s - Drinking water and/or pollution control - E-215. Solid or Hazardous Waste -
E-1209.
Commonwealth of Kentucky, Department for Environmental Protection. Expires
December 31,1998. ID#90060: Oioxin in drinking water.
Maryland Department of Health and Mental Hygiene. Expires September 30, 1998.
Certification #235. Drinking water by Method 1613A.
State of Michigan, Department of Public Health. Expires June 3, 1998. Drinking water by
Method 1613.
Mississippi State Department of Health. No expiration date. Dioxin in drinking water.
Montana Department of Health and Environmental Services. Expires December 31, 1998.
Dioxin in drinking water.
State of New Jersey, Department of Environmental Protection and Energy. Expires June 30,
1998. ID #67851. BNAs and Volatiles. Dioxin in drinking water.
State of New Mexico, Environment Department Recertification pending. Dioxin in drinking
water.
New York State Department of Health. Expires April 1, 1998. ID #11026. Environmental
Analyses of non-potable Water, Solid and Hazardous Waste. Method 1613 in DW.
•
• •
State of North Carolina, Department of Environment Health and Natural Resources Expires
August 31,1999. Certificate # 37751. Djpxin in drinking water.
State of North Carolina, Department of Environment, Health, and Natural Resources,
Division of Environmental Management Expires December 31, 2000. Certificate # 485.
Metals, pesticides & PCBs, semi-volatiles and volatiles; TCLP.
North Dakota State Department of Health and Consolidated Laboratories. Expires
December 31,1998. Certificate # R-076. Effective October 4,1993. Dioxin in drinking water.
Ravfeed 3/2/98 RM
yrcertificVcertiistmem ~
-------
State of West Virginia, Department of Health. Expires December 31, 1998. Certificate No.
9923(C). Dioxin in drinking water.
State of Wisconsin, Department of Natural Resources. Expires August 31,1998. Laboratory
ID Number 999869530, Certification for the following categories off Organics: Purgeabte,
Base/Neutral, Acid, PCBs, and Dioxin. Expires November 14, 1999. Laboratory ID 999869530.
Dioxin in drinking water.
PHARMACEUTICAL
Drug Enforcement Agency (DEA). Expires November 30, 1998. Registration number
RT01195835. Controlled substance registration for schedules 1,2,3,3N,4,5.
N.C. Department of Human Resources. Expires October 31,1998. Registration number
NC-PT 0000 0031. North Carolina controlled substances registration. Application submitted for
renewal.
Food & Drug Administration (FDA) Registration. Expires June 1998. ID #*s 001500 1053481.
Annual registration of drug establishment. Annual registration of drug establishment.
OTHER
Clinical Laboratory Improvement Amendments (CLIA) Registration. Expires May 30, 1999.
ID # 34D0705123. Department of Health & Human Services, Health Care Financing
Administration.
U.S. EPA Large Quantity Hazardous Waste Generator. No expiration date. EPA ID
#NCD982156879. Permit indicates that the laboratory is a large generator of hazardous waste.
North Carolina General License for Radiation Protection. No. expiration date. License No.
032-875-OG. The general license applies only to radioactive material contained in devices which
have been manufactured and labeled in accordance with specific requirements.
Revised 3/2/96 RM «
y:certific\certiistmem V
-------
a
DOCUMENT
CONTROL
Triangle Laboratories, Inc.
801 Capitola Drfv* P.O. Box 13485
Durham, NC 27713*4411 Raaaarch Thkngfo Park. NC 27709-348!
919-544-5729 Fax* 919444-5491
-------
PACIFIC ENVIRONMENTAL SERVICES. INC.
cc>
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Chain of Custody Record
iject Num [Project Name
1012.002 1 US EPA Lima Kiln Screening -Alabama Lima
npton:
Abemathy, Gay, MareL Phoenix, Stegal
Date
3/23/98
3/23/98
3/23/98
3/23/98
3/24/98
3/24/98
3/24/98
3/24/98
3/26/98
3/26/98
3/26/98
3/26/98
3/28/98
3/28/98
3/28/98
3/28/98
*/23/98
3/23/98
3/23/98
Time
Field Sample ID
M23-M-1
M23-I-1-2
M23-I-1-3
M23-I-1-4
M23-I-2-1
M23-I-2-2
M23-I-2-3
M23-I-2-4
M23-I-3-1
M23-I-3-2
M23-I-3-3
M23-I-3-4
M23-M-1
M23-M-2
M23-M-3
M23-I-4-4
M23-O-1-1
M23-O-1-2
M23-O-1-3
Sample Description
Container No. 1 - Filter
Container No. 2 - Train Acetone Rinse
Container No. 3 - Train Toluene Rinse
Container No. 4 - XAD Sorbent Resin
Container No. 1 - Filter
Container No. 2 - Train Acetone Rinse
Container No. 3 - Train Toluene Rinse
Container No. 4 - XAD Sorbent Resin
Container No. 1 - Filter
Container No. 2 - Train Acetone Rinse
Container No. 3 - Train Toluene Rinse
Container No. 4 - XAD Sorbent Resin
Container No. 1 - Filter
Container No. 2 - Train Acetone Rinse
Container No. 3 - Train Toluene Rinse
Container No. 4 - XAD Sorbent Resin
Container No. 1 - Filter
Container No. 2 - Train Acetone Rinse
Container No. 3 - Train Toluene Rinse
Analysis Requested
• A
.w
«3*
^»
o
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
\A
&
S>
CX-
•
•
•
•
•
•
•
•
•
•
*
•
•
•
•
*
•
•
•
Remarks
.
*
4/1/98
Page 1 of 3 Pages
-------
PACinC ENVIRONMENTAL SERVICES. INC.
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919)941-0333 FAX: (919)941-0234
Chain of Custody Record
reject Num project Name
rf)1 2.002 I US EPA Lime Kiln Screening - Alabama Lime
wnplera:
Abemathy, Gay, Marat, Phoenix, Slega)
Date
3/23/98
3/24/98
3/24/98
3/24/98
3/24/98
3/26/98
3/26/98
3/26/98
3/26/98
3/28/98
3/28/98
3/28/98
3/28/98
3/23/98
3/23/98
3/23/98
3/23/98
3/24/98
3/24/98
Time
Field Sample ID
M23-O-M
M23-0-2-1
M23-O-2-2
M23-O-2-3
M23-O-2-4
M23-O-3-1
M23-O-3-2
M23-O-3-3
M23-O-3-4
M23-O-4-1
M23-O-4-2
M23-O-4-3
M23-O-4-4
M23-FB-1-1
M23-FB-1-2
M23-FB-1-3
M23-FB-1-4
M23-FB-2-1
M23-FB-2-2
Sample Description
Container No. 4 - XAD Sorbent Resin
Container No. 1 - Filter
Container No. 2 - Train Acetone Rinse
Container No. 3 - Train Toluene Rinse
Container No. 4 - XAD Sorbent Resin
Container No. 1 - Filter
Container No. 2 - Train Acetone Rinse
Container No. 3 - Train Toluene Rinse
Container No. 4 - XAD Sorbent Resin
Container No. 1 - Filter
Container No. 2 - Train Acetone Rinse
Container No. 3 - Train Toluene Rinse
Container No. 4 - XAD Sorbent Resin
Container No. 1 - Filter
Container No. 2 - Train Acetone Rinse
Container No. 3 - Train Toluene Rinse
Container No. 4 - XAD Sorbent Resin
Container No. 1 - Filter
Container No. 2 - Train Acetone Rinse
Analysis Requested
_t*
§
VJ
-------
u
PACIFIC ENVIRONMENTAL SERVICES. INC.
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919)941-0333 FAX: (919) 941-0234
Chain of Custody Record
oject Mum [Project Name
1012.002 | US EPA Lime Kiln Screening - Alabama Lime
Abemathy. Oay, Maret, Phoenix, Slegal
Date
3/24/98
3/24/98
3/26/98
3726/98
3/26/98
3/26/98
3/27/98
3/27/98
3/27/98
3/27/98
Time
Field Sample 10
M23-FB-2-3
M23-FB-2-4
M23-FB-3-1
M23-FB-3-2
M23-FB-3-3
M23-FB-3-4
M23-RB-1
M23-RB-2
M23-RB-3
M23-RB-4
aHnqulshed by: (Signature)
by: (SAfnature)
fy
Date/Time
Date/Tune
IS$4i ^
Sample Description
Container No. 3 - Train Toluene Rinse
Container No. 4 - XAD Sorbent Resin
Container No. 1 - Filter
Container No. 2 - Train Acetone Rinse
Container No. 3 - Train Toluene Rinse
Container No. 4 - XAD Sorbent Resin
Container No. 1 - Filter
Container No. 2 - Train Acetone Rinse
Container No. 3 - Train Toluene Rinse
Container No. 4 - XAD Sorbent Resin
Received by: (Signature)
Recejyed-forlab bye (Signature)
Analysis Requested
_v,
•o
.
•
•
•
•
•
t
•
•
•
a
o
•
•
•
.
•
•
•
•
•
•
Relinquished by: (Signature)
Date/Time
Remarks
FIELD BLANK 2
FIELD BLANK 2
FIELD BLANK 3
FIELD BLANK 3
FIELD BLANK 3
FIELD BLANK 3
REAGENT BLANK
REAGENT BLANK
REAGENT BLANK
REAGENT BLANK
Received by: (Signature)
REMARKS
4/1/98
Page 3 of 3 Pages
-------
| Custody Seal : Absent Sample Seals: Absent
| Chain of Custody : Present Container...: Intact
| Sample Tag* > Absent
| Sample Tag Numbers: Hot Listed on Chain of Custody
| SHO Forms : N/A
TLI Project Number 45399 Book
Client: PES03 - Pacific Environmental Services ' •
204
Date Received j 04/01/98 j Bv^^ Jff^ *•*<
jj Ice Chest/Box MO COOLANT Carrier and Number j 92
§TLI Number.. ....Client Sample ID Matrix) To I
|mR/H:CPH. Client COC ID * Location | Dat«
| . | ..
AB
/Init
J204-92-1A M23-I-1-1 FILTER) VJ/0
| M23-I-1-1 C02 | Yi/fl-f
(204-92-1B M23-I-1-2 ACETONE RINSE |
| M23-I-1-2 C02 j
| _ ... _ j
J204-92-1C H23-I-1-3 TOLUENE RINSE)
| M23-I-1-3 C02 j
| .) ,.,
J204-92-1D M23-I-1-4 XAD)
jj M23-I-1-4 C02 j
| j
|204-92-2A M23-I-2-1 FILTER)
| M23-I-2-1 C02 |
| ._ _. , ..j
|204-»2-2B M23-I-2-2 ACETONE RINSE)
| M23-I-2-2 C02 j
| j
|204-92-2C M23-I-2-3 TOLUENE RINSE)
| M23-I-2-3 C02 j
| - .,., „.- ._.,,,— . - _ j
|204-92-2D M23-I-2-4 XAD)
| M23-I-2-4 C02 j
| j
|204-92-3A M23-I-3-1 FILTER)
| M23-I-3-1 C02 j
,| . . ... .. . . - ..- j
|204-92-3B M23-I-3-2 ACETONE RINSE)
| M23-I-3-2 C02 |
| _ .... „ .... _„...,, |
|204-92-3C M23-I-3-3 TOLUENE RINSE)
| M23-I-3-3 C02 j
1 1
|204-92-3D H23-I-3-4 XAD)
| M23-I-3-4 C02 j
| , \
|204-92-4A M23-I-4-I FILTER)
| M23-I-4-1 C02 j
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| M23-I-4-2 C02 j /|
.
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ij
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| To LAB
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| To LAB
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-
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Date/Init
•
| To LAB
Date/Init
To STORAGE
Date/Init
— — —
| DISPOSED
Date/Init
1 1
1
1
1 ' |
| Receiving Remarks: ON SAMPLE LABEL:M23-O-l-2, ACETONE HAS MARKED THROUGH AND TOLUENE WRITTEN ABOVE IT; TOLUENE WAS
| ' MARKED THROUGH WITH ACETONE WRITTEN ABOVE FOR SAMPLE M23-O-1-3; NEITHER AGGREBD WITH CLIENT'S COC.
jj Archive Remarks: .1
**
-Form Revised OS/27/1997 -- Page 1 OF 4
-------
RIANCUE LABORATORIES, INC. -- 1,00 IN RECORD/CHAIN OP CUSTODY-
Custody Seal i Absent Sample Seal*; Absent
Chain of Custody i Present Container. . . : Intact
Sample Tags : Absent
Sample Tag Numbers: Not Listed on Chain of Custody
SMO For-* : N/A
TLI Project Number 45399 Book
Client : PES03 - Pacific Environmental Services ' •
204
Date Received j 04/01/98 j Byjff/ / j^t — . — f Page
• i i S^C**SZf *>H*rr~~.
Ice Cheat/Box NO COOLANT Carrier and Number j 92
|TLI Number Client Sample ID Matrix) To I
|mR/H:CPM. Client COC ID * Location | Dat«
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AB
!/Init
|204-92-4C M23-I-4-3 TOLUENE RINSE) V J ., .
j M23-I-4-3 C02 j A^Y/a/*,
1 1 ' '
|204-92-4D M23-I-4-4 XAD)
j M23-I-4-4 C02 j
§|
1
|204-92-5A M23-O-1-1 FILTER)
| M23-0-1-1 C02 1
I 1
(204-92-SB M23-O-1-2 TOLUENE RINSE)
| M23-0-1-2 C02 j
1 I
|204-92-5C M23-0-1-3 ACETONE RINSE)
| M23-O-1-3 C02 j
|204-92-5D M23-O-1-4 XADJ
| M23-0-1-4 C02 j
1 1
|204-92-£A M23-0-2-1 FILTER)
1 M23 -0-2-1 C02 j
1 1
1 1
|204-92-6B M23-O-2-2 ACETONE RINSE)
jj M23-0-2-2 C02 j
|204-92-6C M23-O-2-3 TOLUENE RINSE)
1 M23-0-2-3 C02 j
1 1
|204-92-6D M23-0-2-4 XAD|
| M23-0-2-4 C02 j
1
|204-92-7A M23-0-3-1 FILTER)
| M23-0-3-1 C02 j
1 1
|204-92-7B M23-0-3-2 ACETONE RINSEJ
| M23-0-3-2 C02 j
1
1 1
|204-92-7C M23-0-3-3 TOLUENE RINSE)
| M23-0-3-3 C02 j
|204-92-7D M23-0-3-4 XAD) Jj^
| M23-0-3-4 C02 j «^* J
fyf.
To STORAGE
Date/Init
J
^
(M
*t
| To LAB
Date/Init
To STORAGE
Date/Init
| To LAB
Date/Init
To STORAGE
Date/Init
•
| To LAB
Date/Init
•
To STORAGE
Date/Init
| DISPOSED
Date/Init
•
•
| Receiving Remarks: ON SAMPLE LABEL:M23-O-l-2, ACETONE HAS MARKED THROUGH AND TOLUENE WRITTEN ABOVE IT; TOLUENE HAS
| MARKED THROUGH WITH ACETONE WRITTEN ABOVE FOR SAMPLE M23-O-1-3; NEITHER AGGREED HITH CLIENT'S COC.
1
| Archive Remarks: <•
•Form Revised.-05/27/1997 -- Page 2 OF 4=
...-.lit. fit',:'
-------
| Custody Seal : Absent Sample Seals: Absent
| Chain of Custody : Present Container. . . : Intact
| Sample Tags i Absent
| Sample Tag Numbers: Not Listed on Chain of Custody
| SHO Forms t N/A
TLI Project Number 45399 | Book
Client > PES03 - Pacific environmental Services ' |
, ' j 2M
Date Received \ 04/01/98 j *Y$yS ^ ,*2&~~" I p"9*
1 Ice Chest/Box _ NO COOLANT Carrier and Number j ' 92
|TLI Number Client Sample ID Matrix) To
|oR/H:CPM. Client COC ID • Location | Dat
LAB
e/Init
|204-92-8A M23-0-4-1 FILTERJ jj/j
jj M23-0-4-1 C02 | "till/of
|204-92-8B M23-O-4-2 ACETONE RINSE)
| M23-0-4-2 C02 j
|204-92-8C M23-0-4-3 TOLUENE RINSE)
| M23-0-4-3 C02 j
1 I
|204-92-0D M23-O-4-4 XAD)
| M23-0-4-4 C02 j
1 1
|204-92-9A M23-FB-1-1 FILTER)
| M23-FB-1-1 C02 j
II
|204-92-9B M23-FB-1-2 ACETONE RINSE)
| M23-FB-1-2 C02 j
1 1
|204-92-9C M23-FB-1-3 TOLUENE RINSE)
| • H23-FB-1-3 C02 j
|204-92-9D M23-FB-1-4 XAD)
| M23-FB-1-4 C02 |
|204-92-10A M23-FB-2-1 FILTER)
| M23-FB-2-1 C02 j
I j
•1 i
|204-92-10B M23-FB-2-2 ACETONE RINSE)
| M23-FB-2-2 C02 j
1
|204-92-10C M23-FB-2-3 TOLUENE RINSE)
| M23-FB-2-3 C02 j
|204-92-10D M23-FB-2-4 XAD|
| M23-FB-2-4 C02 j
|204-92-llA M23-FB-3-1 FILTER)
| M23-FB-3-1 C02 j
1 j ^
|204-92-llB M23-FB-3-2 ACETONE RISE) ty j) 1
| M23-FB-3-2 C02 1 1 Ml f\
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Date/Init
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/
/
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| To LAB
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,
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Date/Init
| To LAB
Date/Znit
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Date/Init
-
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Date/Init
•
-
To STORAGE
Date/Inie
I
| DISPOSED
Date/Init
•
•
I Receiving Remarks: ON SAMPLE LABEL:M23-O-l-2, ACETONE HAS MARKED THROUGH AND TOLUENE WRITTEN ABOVE IT; TOLUENE HAS
| MARKED THROUGH WITH ACETONE WRITTEN ABOVE FOR SAMPLE M23-O-1-3; NEITHER AGGREED WITH CLIENT'S COC.
1
| Archive Remarks:
-Form Revised 05/27/199? -- Page 3 OF 4
-------
aTRIANGLE LABORATORIES, INC. -- LOG IN RECORD/CHAIN OF CUSTODY-
Custody Seal : Absent Sample Seals: Absent
Chain of Custody t present Container...: Intact
Sample Tags : Absent
Sample Tag Numbers: Not Listed on Chain of Custody
SHO Forms > N/A
TLI Project Number 4S399 | Book
Client: PES03 - Pacific Environmental Services ' {
204
t |
Date Received j 04/01/98 j By /£. S ^£^-"-"*d""p«ae
s i / Lft/lt jfTUl**^ A
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|TLI Number Client Sample ID Matrix
|mR/HtCm. Client COC ID * Location
|204-»2-llC M23-PB-3-3 TOLUENE RINSE
M23-FB-3-3 C02
204-92-11D M23-PB-3-4 XAD
M23-FB-3-4 C02
204-92-12A M23-RB-1 FILTER
M23-RB-1 C02
204-92-12B M23-RB-2 ACETONE RINSE
M23-RB-2 C02
204-92-12C M23-RB-3 TOLUENE RINSE
M23-RB-3 C02
204-92-12D M23-RB-4 XAD
M23-RB-4 C02
| To LAB
Date/lnit
Ml
fol*f
A/I
" iftlW
1
To STORAGE
Date/lnit
vVl
u
iJ
-
| To LAB
Date/lnit
To STORAGE
Date/lnit
| To LAB
Date/lnit
-
To STORAGE
Date/lnit
•
| To LAB To STORAGE
Date/lnit Date/lnit
•
DISPOSED
Date/Init
•
Receiving Remarks: ON SAMPLE LABEL:M23-O-l-2, ACETONE HAS MARKED THROUGH AND TOLUENE WRITTEN ABOVE IT; TOLUENE HAS
MARKED THROUGH WITH ACETONE WRITTEN ABOVE FOR SAMPLE M23-O-1-3; NEITHER AGGREED HITH CLIENT'S COC.
Archive Remarks:
•Form Revised 05/27/1997 -- Page 4r-OF 4<
-------
TRIANGLE LABORATORIES, INC.
SAMPLE TRACKING AND PROJECT MANAGEMENT FORM
TLI Proj#: 45399-
Prod Code: D23451
DetectLim: 0.05 ng
-ADMINISTRATIVE INFORMATION---
Samples: 12 TurnAround.: 21 Day(s)
Matrix.: M23 Hold Time..: 30 Day(s)
Type...: A Start Date.: 04/02/98
Recvd..: 04/01/98 Ship By : 04/21/98
DWL Due Dt.: 04/09/98
Analyte List.: Tetra-Octa CDDs/CDFs
Method : Method 23: T-O, Toluene Combined
Client Proj..: r012.002/Lime Kiln
Client : Pacific Environmental Services (PES03)
P.O. No : 104-98-0159 Collect Dt/Tm: SeeCOC
Contact : Mike Maret Phone : 919-941-0333
Proj . Mgr. . . . : Rose West Fax : 919-941-0234
Sample Origin: AL
SPECIAL INSTRUCTIONS / QA REQUIREMENTS
Prep Project: 04228 Prespike Standard: USF-CS
Prespike Amount..: 4.Ong
Extraction Exp...: 04/22/98
REPORTING REQUIREMENTS-
Reporting Format: Report Option II
See MILES for Instructions/Communications.
Completed by:
Reviewed by:
DATE:
DATE:
(PMGT0197)
-------
' PROJECT COMMUNICATION TRACKING FORM
TU Project Number 453*7 .-
Use this form to record afl exchanges of information between production units as well as personnel
handling this project Decisions, corrective actions and recommendations must also appear on this
tracking document
Name
Comment / Decision / Resolution / Action / Observation
PES03-Pacif1c Environmental Services
M23-I-3-4
P i-oj ©c-t : -4-5399
2O-4-—92 —3D
-/Habama Lime - R012.002
toe. '—*
Morth Carolina
module
Triar.aI-5
TLI PaOJ
0422S
DATE: ••.;r-"r-(:>:
SPIKS 'USFTC -:« us?-;;
PREPSI '• *• ' AC
PAOIJIC SNViaOSMi
PESOS-Pacific Environmental Services
M23-I-4-4
O 4-— 9 "2. — *• O
/US EPA Ume Kki Screening - AtatyS%l3fe*|KipB
i Pacific EnvfeaoMNMSOTtoes, tot
•Research Triangle Park, North
\MunNok
:nc.
-T- 93-17-98
& USF-S
ENVIRONMENTAL
j£t
-------
PESOS-Pacific Environmental Services
M2 3-0- 1-4
— 92— 5D
US &A Urn Mh Screening - Alabama Lime - R012.002
jiviroronenta* Service* *»
. North Carolina
-1-4 XAD sorbent moduJa
Triangls Laboratories, Inc.
TLI PROJECT #04228
DATS: 03-17-98
SPIKE: USFrC & USF-S
3PIKER «lir
PREF2D BT^AC
PACIFIC ENVIRONMENTAL
PESOS-Pacific Environmental Services
M23-0-2-4
P^^ f~\ "i -*""*• /•••» •+" «• ^l_ Ct G} Gk
• V-** ^J ^y v^,* Cx « ^^ ^w1 *-? ^? 5^
20-4-— 92— 6D
t
V S^.?^ ^me ^"° Screen«g- Alabama Lime - R012 002
i. Paqpc Entrirenmentat Saivices* Ite.
f Research Triangle Park, North
/ Run No. M23-O-3
iJ>B*ttoWr Not. MlVOi2-4 XAD i
Triangle Laboratories, Inc.
TLI PROJECT #04223
DATE: 03-17-98
SPIKE: USF-rC & USF-S
SPIKER ''frjBfo.V
PREPED BY AC ' ' x . '
PACIFIC ENVIRC!.'M^rPTAL
000-
Tnangie Laboratories, inc
TLI PROJECT #04228
DATE: 03-17-98 TLI BLANK
SPIKE: aSF-C & USF-S
SPIKER
,PREPED BY AC
PACIFIC ENVIRONMBMTAL
17
-------
PROJECT COMMUNICATION TRACKING FOflM
page of
TU Project Number:
f 1
Use this form to record all exchanges of information between production units as well as personnel
handling this project Decisions, corrective actions and recommendations must also appear on this
. ' ' tracking document.
Date
Name
Comment / Decision / Resolution / Action / Observation
is ,
,,
£
'^1-74 0 A'lfcr
f , , & , \
\ le**ait Jfr 6 /
-a
2o*l-*2-5fi. 0
.X/VD
( >*~,
"2A 9 ^'1^^ Of*~\ P0y^«- (CA K jkr)
Ma. C2M19*
ATTACHWINri
toMe»»mo«f ma
-------
' PROJECT COMMUNICATION TRACKING FORM
TU Project Number:
Use this form to record all exchanges of information between production units as well as personnel
handling this project. Decisions, corrective actions and recommendations must also appear on this
. • ' tracking document
Date
Name
Comment / Decision / Resolution / Action / Observation
~ l/t-
V
^J
/7#*rtL+.-&J, J <
OP No.
ATTACMMCNrt
. to
-------
Date: 04/03/9B
Times 11:41
Sample
* crd TU_Number.. Customer.Sample. Id
000 TLI Blank TLI M33 Blank
001 204-92-1A-D M23-I-1
002 204-92-2A-D M23-I-2
003 204-92-3A-D M23-I-3
004 204-92-4A-D H33-I-4
005 204-92-SA-D H23-0-1
006 204-92-6A-D M23-0-2
007 204-92-7A-D M23-O-3
00( 204-92-8A-O H23-0-4
009 204-92-9A-D M23-FB-1
010 204-92-10A-D H23-FB-2
Oil 204-92-11A-D M23-FB-3
012 204-92-12A-D M23-RB-1-4
013 TLI LCS TLI LC8
014 TLI LCSD TLI USD
TRIANGLE liABUKAIUKjto, in\..
Wet Lab MM5/PUF Observations
Project: 45399
P.
No
0
1
1
1
1
1
1
1
1
1
1
1
1
0
0
XAD
Color
WHITE
WHITE
WHITE
WHITE
WHITE
WHITE
WHITE
WHITE
WHITE
WHITE
WHITE
WHITE
WHITE
WHITE
WHITE
Filter
Color. .
HA
OREY
GREY
GREY
BROWN
WHITE
WHITE
GREY
GRAY
WHITE
WHITE
WHITE
WHITE
NA
HA
Glass We
NA
WHITE
WHITE
WHITE
WHITE
WHITE
WHITE
WHITE
WHITE
WHITE
WHITE
WHITE
WHITE
NA
NA
)0l PUF
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
. . . . Odor. .
NONE
NONE
NONE
NONE
NONE
NONE
NONE
NONE
NONE
NONE
NONE
NONE
NONE
NONE
NONE
Air
Q.No
0422S
04226
04228
0422S
04228
04228
04228
04228
04228
04228
04228
04228
04228
NA
NA
Entered By
WHIGHAM
WHIGHAM
WHIGHAM
WHIGHAM
WHIGHAM
WHIGHAM
WHIGHAM
WHIGKAM
WHIGHAM
WHIGHAM
WHIGHAM
WHIGHAM
WHIGHAM
WHIGHAM
WHIGHAM
Date
04/03
04/03
04/03
04/03
04/03
04/03
04/03
04/03
04/03
04/03
04/03
04/03
04/03
04/03
04/03
10:59
10:59
10:59
10 1 59
10:59
10:59
10:59
10:59
10:59
10:59
10:59
10:59
10:59
10:59
10:59
Time. .
P
P
P
P
P
P
P
P
P
P
P
P
P
P
P
. s
*•• End of Report ***
-------
Project: 45399
TRIANGLE LABORATORIES, IMC. PAGE 1 OF 2
Dioxin Sample Preparation Tracking 4 Management Form
Client: Pacific Environmental Services (PES03)
Solvent (s)/Acid(s) :
Lot Numbers:
IS Spike: 40 vl cone: 0.1000 ng/jil
EA>fH-?/
Method: Method 23: T-0, Toluene Combined Matrix:
Extraction Date: CH /O?/9Sf
SS Spike: «1 cone: . nq/ul
MS Spike: 0 Ml cone: 0.0000 ng//tl
LCS Spike: 0 ni cone: 0.0000 ng/pl
OPR Spike: 20 ;il cone: _0.01 ng/jil
| TLI / | GROSS | SA
S#.crd| SAMPLE / CLIENT | HEIGHT | S
| ID / SAMPLE ID | Before After | &-
\ TLI Blank | I I
000 | TLI M23 Blank | - | ~" ~~" |
| 204-92-1A-D | | ^ |
001 | M23-I-1 | " | |
| 204-92-2A-D | __ | |
002 | M23-I-2 | | |
| 204-92-3A-D | | |
003 ! M23-I-3 | 1 "^ 1
| 204-92-4A-D | | |
1004 | M23-I-4 | | |
! | 204-92-5A-D | . | |
|005 | M23-0-1 | | ' " |
| | 204-92-6A-D | I |
|006 | M23-0-2 | ~ | * |
| | 204-92-7A-D | | |
(007 | M23-0-3 | | |
| | 204-92-8A-D | | |
|OOB | M23-0-4 | | ' |
| | 204-92-9A-D | | |
|009 | M23-FB-1 | | ' |
| "JW | \W /«-<" I JP/r IChemirt
i *0/Y& i S4*> T *«/vr i C#p5 ISP*. *
i tsT-J: i uiF-iM 05P-C5 i (Kt*'A i • n>
\ */rf/Vb\ il/ «L& JL / *?/_?? 1 M 1 £. l&\ " Expir
„ O*/ / n tff I tfV / P3/t5 O*( / 65 /tt\ (4 1 d /ff \ • Date
MPLE | 1L : JOt^J jfL • Ji«-Vl JL •• A-U M ' =L£ I ' Time
IZE | 6- 1 ng/Ml | 0-01 ng/»l _£j_ng/|il 1 t>* ! os/ui \ • Cone.
A-»i.| % Ml 1 Vo «1 1 VO «1 I IfO jil I • Vol.
J 1 ! | tftny Leftt
i i
. . +. .-C>^tyx* + +.jV(?:...^ *
|| | |Any Left|
i <£^ " i5i5/K «^s<8)
| | | | [Any Left|
1 5.i4rv^ ' ' ' Str l ye3^1
| | | | |Any Left|
\ i ^S^ i i 1 4#/i~- i »~<£i
it 1 1 1 l*ny Leftl
1 ' 5^rvx ' 'i5yn |yea^'
\ | | | |Any Left
1 1 5^ . 1 1 ^ i ye.^
\ 1 1 | |Any Left
! ^$K 1 1 Jfa 1 -s^
1 1 1 1 Iftny i**t
1 ' ^^! ! [Jtf/^ \y"&
ill | [Any Left
1 . 5^. , i^~iv<9
.1.1 1 1 , (Any Left
1 i S^r^ i i i Co^v i y«^a)
I Gross weight of sample container * sample before/after aliquot removal.
I
Comments:
Initial*:
Date:
of both SPIKER AND OBSERVER muat be entered.
XXXZX - Gross Height not provided for WATER Sample*.
REV OS/J7/97 (PSTMF 7)«-
-------
TRIANGLE LABORATORIES. OK. PAGE 2 OF 2
Dioxin Sample Preparation Tracking ft Management Fora
Project: 45399 Client: Pacific Environmental Services (PBS03)
Solvent (a) /Acid (s) : *W\f.*Kr / / Method: Method 23: T-O. Toluene Combined
Lot Numbers: tfjfd |^*fH"^/ 1 Extraction Date: *^/ C/ fa
i
SS Soike: ul cone: . ng/«l | /^ ' /'•H/ | / frW |
MS Spike: 0 pi cone: 0.0000 ng/pl | 06 /V 6 | 5"67* T | 5"tUf/F |
LCS Spike: 0 pi cone: 0.0000 na/ul | "5P -JT | *S$ f?-t+t \ t/5P-C3 |
OPR Spike: 20 pi cone: _0.01 ng/pl 1 IZ / *j{ /Q \ & / *L /?* 1 JL / Qi fll 1
I 1 TLI / I GROSS | SAMPLE | U : lbft.fl,, H : 1 ^n. jL. l\ : .2 lfr..4~
|S».crd| SAMPLE / CLIENT | HEIGHT | SIZE | &7 nq/itl | *« nq/pl | _0j_ng/pl |
| | ID / SAMPLE ID 1 Before After 1 .* t mi 1 V« «1 1 «/0 B! 1 Vo «1 |
| | 204-92-10A-D 111(1 1 1 1
1010 | M23-FB-2 I ~" I ~ I ' I -5^^ ' ' '
| | 204-92-llA-D | | | | | I |
|011 | M23-FB-3 | | | 1 | <^ /. | | |
' O«^v\
| | 204-92-12A-D 1 1 1 . 1 1 1 1
|012 | M23-RB-1-4 | | — | j | ^ ' ^{jtV^
\ TLI LCSD | | '|'//J ' ^ ' '
|014 | TLI LCSD | "~ I l| O'PP1^- ' <^A- ' ^ ^ '
1 1 1 1 1 1 1 1
1 1 1 1 1 1 1 1
1 1 1 1 1 1 1 1
1 1 1 1 1 1 1 1
1 1 1 1 1 1 1 1
1 1 1 1 1 1 1 1
1 1 1 1 1 1 1 1
1 1 1 1 1 1 1 1
1 1 1 1 1 \ \ 1
1 1 1 1 1 1 1 1
Matrix: ^T^jP
5*"*^ IChemii
$7&T> % ISpike
I/IF '-$ i • ID
Ml A l^\ ' Ex,
•• : | " Til
0,1 nq/iil | • Cea
iff «i I • vo:
y [Any L<
|Any Li
|Any L
VVv~^ ' yes^
[i^jiy L
S^Jr-^ 1 yes*
|Any L
1 yes/
|Any I
1 yes/
|Any I
1 yes/
|Any I
1 yes/
|Any 1
1 yes;
ross weight of sample container + sample before/after aliquot removal
2 i
mrnents:
k/
72 u
Initials:
Date: I.I.
it both SPIKER AND OBSERVER oust be entered.
Qrosa Height not provided for HATER Sampl
- REV 05/27/97 (PSTMP
-------
-------
PAGE 2 OP 2
TRIANGLE LABORATORIES. INC.
DIOXIN SAMPLE EXTRACTION and CLEANUP TRACKING FORM
TLI Project No.: 45399
••+•
* i 1
Ext Stt.crd and
TLI Number |
mmmmmmmmmmmmmmmmmm-¥
010
204-92-10A-D
I
I
I
I
I
Enter the procedure number below into the box at the top of each column to signify the step performed.
Initial and date each sample for each numbered procedure performed.
# PROCEDURE SOP.#. .v. . DETAILS (circle)
(l) EXTRACTION Time On : Time Off :
Jar / Sep Funnel / Steam Dist / Cont LL / ASE / Haste Dilution
SPIKE AFTER EXT'N
ADD TRIDECANE Lot#_
ROTOVAP /"Z. I <£ 40mL
COMBINE
^TVVLIP. DETERM. 20%/80% (So%/S0%\ 5mL/20mL Other_
SOLVENT EXCHANGE Iso-Octane Lottt ^7/7/^1 Heptane Lot#_
Qj> CLEANUP N/ .S ^SP 26
(Q TRANSFER
10} ADDITIONAL CLEANUP
11) FINAL TRANSFER
/ DSP 225 / DSP 115 / DSP 215 / DSP 267 / Other
Mod. DSP 260 / DSP 225 / DSP 115 / DSP 215 / DSP 267 / DSP260 ClOg)
Comments:
•«Rev 11/25/S7 (PSTMF
I
-------
PAGE 1 OF 1
TRIANGLE LABORATORIES, INC.
Transfer Chain-of-Custody Form
Project 45399
Transfer From: DWLH5 To: DMS5
Released by:
Accepted by:
MILES .ID
45399- -000
45399- -001
45399- -002
45399- -003
45399- -004
45399- -005
45399- -006
45399- -007
45399- -008
45399- -009
45399- -010
45399- -Oil
45399- -012
45399- -013
45399- -014
Initials . .
4-
\JO\-
TLI No
TLI Blank
204-92-1A-D
204-92-2A-D
204-92-3A-D
204-92-4A-D
204-92-5A-D
204-92-6A-D
204-92-7A-D
204-92-8A-D
204-92-9A-D
204-92-10A-D
204-92-11A-D
204-92-12A-D
TLI LCS
TLI LCSD
Date Time ,. . .
\1_/
-------
PAGE 1 OF 2
Method: Method 23: T-0. Toluene Combined
Required Detection Limit: 0.05 ng
TRIANGLE LABORATORIES. INC.
HR GC/BRMS ANALYSIS
(PROJECT: 4S399
SAMPLE INFORMATION
1ST COLUMN
2ND COLOMN
RS Cone
20 ni • 100.0
1 1
ISf.crdj
1 1
1 1
(000 |
1 1
(001 |
1 1
(002 |
1 1
(003 |
1 1
|004 |
1 1
|005 |
1 1
(006 |
1 I
|007 |
1 1
|008 |
1 1
(009 |
1 1
(010 |
1 1
(oil 1
TLI / | GC/MS FILENAME (CONFIRM (CONFIRM FILENAME | OSF-RS
SAMPLE ID / CLIENT 1 COLQtW: ^.j 1 ICOLUMN: 9A&*f' IVOUM
/ SAMPLE ID | (1 (SOLN I
(OSF-RS (ANALYSIS
E IINIT. (COMMENTS
•D (DATE |
TLI Blank | | | | &0 <£ | Pn/ |
TLI M23 Blank | -s/7 T ' ty*' 1 P^'3tl3&f' \f » l0^ I \l | 0<, 7 |
204-92-8A-D | 1
-------
PAOS 2 OF 2
Method: Mechod 23: T-0. Toluene Combined
Required Detection Limit: 0.05 ng
TRIANGLE LABORATORIES. INC.
HR GC/HRMS ANALYSIS
JPROJECT: 45399
SAMPLE INFORMATION
1ST COLUMN 2ND COLUMN
RS Cone
20 pi • 100.0 FO/jil
| TLI / | GC/MS FILENAME |CONFIRM (CONFIRM FILENAME JOSF-RS
#.crd| SAMPLE ID / CLIENT | COLUMN: | I COLUMN; *Pft?t) (VOLUME
| / SAMPLE ID | || I SOLS ID
IOSF-RS (ANALYSIS
IINIT. |COMMENTS
(DATE |
113
204-92-12A-D |
M23-RB-1-4 |
TLI LCS
TLI LCS
I
I
I
114
TLI LCSD
TLI LCSD
\Ttt>jP I
Comments:
Type: A
Spike File: SPMIT204 |
I
Amt of Extract: 50% i
---REV 03/07/95 (PSTMF 6)--i
27
-------
rwn uug
Instrument IP
Column Type Column ID plot Name Ini. Vol. Acquisition
OL^— -
Signature
G/C
M/.yrtl
Date
Transcribed from chromatographic data
Dated initials required
s(vr1/qa/formsAirrunlog.doc (02/05/97)
1 ^t *
ConCal Due:
ConCal Due:
Page:.
-------
many IB uauutaiuuoa,
Run Log '
Transcribed from chromatographic data
»* Dated initials required
Brvr1/qa/forms/hnunlofl.doc (02/05/97)
n«ia:
Page:
-------
Plot Name
775A
Transcribed from chromatographic data
** Dated initials required
srvr1/qaflbmw/hmmlog.doc (02/05/97)
ConCal Due:
ConCal Due:
-------
i nangie Laooraiones, inc.
Run Log
Transcribed from chromatographic data
** Dated initials required
8rvr1/qa/lbrm8/hrrunlog.doo (02/0587)
ConCal Due:
ConCal Due:
: ' f
-------
Instrument ID
IMA
Transcribed from chromatographic data
» Dated Initials required
«vr1/qa/fonn«/hmmlog.doc (02/05W7)
ConCal Due: //O.Y)pr»v
-------
Triangle Lr*v>raiories,
f Log
Instrument ID Column Type
Column IP
Plot Name
Acouisilion
M H
1(111 U.u.
Signature
G/C
Comments**
Transcribed from chromatographic data
•* Dated initials required
srvM/qa/formB/hrrunlog doc (02/05/97)
ConCal Due:
ConCal Due:
3fc
-------
Run Log
Instalment ID Column Type Column ID p|ot Name
\i Or~~T-O V^) \^&* x~ &6? *Vi 1 T T CD \_
Ini. Vol. Acauisition
v.0,^ ftofr^oS
G/C
)opns- oj1
U\_ 4/;r/«
Signature
Date
Filename
Date*
Time*
Project*
Sample*
No.
Client Sample ID
Syr
332
Operator/Date
Comments*
k^i
QtV^ M|if»
u
- t)
e> I
-14-
•2:
PS-
> -1 4-
7.
^ c
c
HVb-I -
- j: -
<*-()
* Transcribed from chromatographic data
** Dated initials required
sivrl/qa/forms/hmjntog.doc (02J05/97)
ConCal Due:
ConCal Due:
Page:
20
-------
Triangle Laboratories, Inc.
Run Log
Instrument IP
TOP
Column Tvoe
~b/?2Z 5 "
Column ID Plot Name
Inj. Vol.
Acquisition
QIC
Date
Filename
Date*
Time*
Project #
Sample*
No.
Client Sample ID
Syr
332
Operator/Dale
Commenls*
C 9'r
f*?t(lo3
fir 1
--
IMJL
I8j*_
rr
•*•* Ml>~0~ 1
HI,
7-
lHi
if
Transcribed from chromatographic data
Dated initials required
ConCalDue:
ConCalDue:
-------
Triangle Laboratories, Inc.
Run Log
InsfrMmentlP £ojumnTvpe Column ID pjot Name
"lo f? C}£ 1 1 f -^ j c?o i S "f *f f
inj. Vol. Acquisition
C **i>5C t ^
j
Signature
G/C
^V^'^v^
Lf/ 1 bf*?Z
1 Dfle
Transcribed from chromatographic data
** Dated initials required
%8ivr1/qa/form8/hminlog.doc (02/OW97)
ConCal Due:
ConCal Due:
36
15
-------
SAMPLE
DATA
Triangle Laboratories, toe.
801 Capitota Drive P.O. Box 13485
Durham, NC 27713-4411 ttueerch Triangle f
919-5444729 fax $919-844*8491
IH «C 2770*3485
37
-------
Data File
Sample ID
Units
Extraction Date
Analysis Date
Instrument
Matrix
Extraction Type
Analytes
2378-TCDD
12378-PeCDD
123478-HxCDD
123678-HxCDD
123789-HxCDD
1234678-HpCDD
OCDD
2378-TCDF
12378-PeCDF
23478-PeCDF
123478-HxCDF
123678-HxCDF
234678-HxCDF
123789-HxCDF
1234678-HpCDF
1234789-HpCDF
OCDF
TOTAL TCDD
TOTAL PeCDD
TOTAL HxCDD
TOTAL HpCDD
TOTAL TCDF
TOTAL PeCDF
TOTAL HxCDF
TOTAL HpCDF
TRIANGLE LABORATORIES OF RTP, INC.
Sample Result Summary for Project 45399
Method MIT2 Analysis (DB-5)
==============================================
U980780 W981017 W981018
TLI M23 Blank M23-I-1 M23-I-2
ng
04/03/98
04/15/98
U
XAD
Soxhlet
(0.002)
(0.002)
(0.003)
(0.002)
(0.002)
(0.003)
0.01 J
{0.004}J
(0.002)
(0.002)
(0.002)
(0.002)
(0.002)
(0.002)
(0.002)
(0.002)
(0.003)
(0.002)
(0.002)
(0.002)
(0.003)
{0.004}
(0.002)
(0.002)
(0.002)
ng
04/03/98
04/16/98
W
M23
Soxhlet
(0.03)
(0.05)
(0.06)
(0.06)
(0.06)
(0.09)
(0.1)
0.05
(0.03)
(0.04)
(0.04)
(0.04)
(0.04)
(0.05)
(0.06)
(0.08)
(0.1)
(0.03)
(0.05)
(0.06)
(0.09)
0.09
{0.06}
(0.04)
(0.06)
ng
04/03/98
04/16/98
W
M23
Soxhlet
B
Other Standards Percent Recovery Summary (% Rec)
37C1-TCDD 87.9 83.3
Other Standards Percent Recovery Summary (% Rec)
13C12-PeCDF 234 106
13C12-HXCDF 478 108
13C12-HXCDD 478 114
13C12-HpCDF 789 90.1
89
78.
75,
83.6
Other Standards Percent Recovery Summary (% Rec)
13C12-HXCDF 789 84.5 82.4
13C12-HxCDF 234 81.8 114
Internal Standards Percent Recovery Summary (% Rec)
13C12-2378-TCDF 65.8 71.2
13C12-2378-TCDD 67.9 78.1
(0.04)
(0.07)
(0.09)
(0.08)
(0.08)
(0.1)
{0.29}
1.5
0.21
0.21
0.10 J
{0.05} J
(0.06)
(0.07)
{0.05} J
(0.1)
(0.1)
0.25
{0.11}
0.07
(0.1)
12.1
2.7
0.33
{0.05}
84.7
88.8
81.0
75.6
85.1
90.3
78.2
73.1
74.0
Page 1
04/21/98
T981957
M23-I-3
ng
04/03/98
04/18/98
T
M23
Soxhlet
(0.003)
(0.004)
(0.007)
(0.007)
(0.007)
(0.01)
{0.03} JB
0.02 B
(0.003)
(0.003)
{0.007}J
{0.004}J
(0.004)
(0.005)
0.009 J
(0.008)
(0.02)
0.01
(0.004)
(0.007)
(0.01)
0.11
0.02
0.01
0.009
84.9
94.9
87.6
90.8
68.1
80.1
94.0
76.6
71.7
Triangle Laboratories, Inc.® Analytical Services Division
801 Capitola Drive • Durham, North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 11:23 04/21/91
-------
TRIANGLE LABORATORIES OF RTF, INC. Page 2
Sample Result Summary for Project 45399 04/21/98
Method MIT2 Analysis (DB-5)
Data File U980780 W981017 W981018 T981957
Sample ID TLI M23 Blank M23-I-1 M23-I-2 M23-I-3
Units ng ng ng ng
Extraction Date 04/03/98 04/03/98 . 04/03/98 04/03/98
Analysis Date 04/15/98 04/16/98 04/16/98 04/18/98
Instrument U W W T
Matrix XAD M23 M23 M23
Extraction Type Soxhlet Soxhlet Soxhlet Soxhlet
Internal Standards Percent Recovery Summary (% Rec)
13C12-PeCDF 123 68.6 68.5 64.9 72.6
13C12-PeCDD 123 99.4 71.8 68.3 80.1
13C12-HxCDF 678 68.1 119 87.9 101
13C12-HxCDD 678 78.7 115 93.0 93.2
13C12-HpCDF 678 83.7 115 100.0 99.8
13C12-HpCDD 678 92.5 116 107 101
13C12-OCDD 83.0 103 95.4 65.6
Triangle Laboratories, Inc.® Analytical Services Division
801 Capitola Drive • Durham, North Carolina 27713 Printed: 11:23
Phone: (919) 544-5729 • Fax: (919) 544-5491
-------
Data File
Sample ID
Units
Extraction Date
Analysis Date
Instrument
Matrix
Extraction Type
Analytes
2378-TCDD
12378-PeCDD
123478-HxCDD
123678-HxCDD
123789-HxCDD
1234678-HpCDD
OCDD
2378-TCDF
12378-PeCDF
23478-PeCDF
123478-HxCDF
123678-HxCDF
234678-HxCDF
123789-HxCDF
1234678-HpCDF
1234789-HpCDF
OCDF
TOTAL TCDD
TOTAL PeCDD
TOTAL HxCDD
TOTAL HpCDD
TOTAL TCDF
TOTAL PeCDF
TOTAL HxCDF
TOTAL HpCDF
TRIANGLE LABORATORIES OF RTP, INC.
Sample Result Summary for Project 45399
Method MIT2 Analysis (DB-5)
T981958
M23-I-4
ng
04/03/98
04/18/98
T
M23
Soxhlet
(0.003)
(0.004)
(0.006)
(0.005)
(0.005)
0.008 J
Page 3
04/21/98
0.04
0.34
0.04
0.04
0.01
0.008
0.008 J
(0.004)
0.007 J
(0.007)
(0.02)
0.02
{0.003}
0.01
0.02
2.6
0.38
0.05
0.007
JB
T981959
M23-O-1
ng
04/03/98
04/18/98
T
M23
Soxhlet
(0.01)
(0.02)
(0.02)
(0.02)
(0.02)
(0.03)
(0.05)
{0.02} B
(0.01)
(0.01)
(0.01)
(0.01)
(0.01)
(0.01)
(0.02)
(0.02)
(0.04)
0.03
(0.02)
(0.02)
(0.03)
{0.02}
{0.01}
(0.01)
(0.02)
T981960
M23-0-2
ng
04/03/98
04/18/98
T
M23
Soxhlet
(0.006)
(0.009)
(0.01)
(0.01)
(0.01)
0.01 J
{0.03} JB
0.03 B
(0.006)
(0.006)
(0.008)
(0.007)
(0.009)
(0.01)
{0.01} J
(0.02)
(0.03)
0.08
0.03
(0.01)
0.01
0.25
0.02
{0.007}
{0.01}
=======
Other Standards Percent Recovery Summary (% Rec)
37C1-TCDD 88.9 92.6
Other Standards Percent Recovery Summarv (% Rec)
13C12-PeCDF 234 96.0 107
13C12-HXCDF 478 92.2 91 3
13C12-HXCDD 478 93.2 99*4
13C12-HpCDP 789 76.0 84!8
Other Standards Percent Recovery Summarv (% Rec)
13C12-HxCDF 789 76.1 38 5 V
13012-HxCDF 234 75.6 39^2 V
Internal Standards Percent Recovery Summarv (% Rec)
13C12-2378-TCDF 60.6 229 V
13C12-2378-TCDD 53.7 22!3 V
87.1
98.8
91.0
95.9
82.2
66.8
73.2
57.4
54.3
S982305
M23-0-3
ng
04/03/98
04/18/98
S
M23
Soxhlet
(0.006)
(0.009)
(0.01)
(0.01)
(0.009)
(0.01)
(0.02)
{0.007}JB
(0.006)
(0.006)
(0.006)
(0.006)
(0.007)
(0.008)
(0.01)
(0.01)
(0.01)
(0.006)
(0.009)
(0.01)
(0.01)
{0.007}
(0.006)
(0.007)
(0.01)
96.7
102
97.4
96.5
95.2
62.9
65.3
54.8
49.0
Triangle Laboratories, Inc.® Analytical Services Division
801 Capitals Drive • Durham, North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 11:23 04/21/91
4
-------
TRIANGLE LABORATORIES OF RTF, INC.
Sample Result Summary for Project 45399
Method MIT2 Analysis (DB-5)
Data File
Sample ID
Units
Extraction Date
Analysis Date
Instrument
Matrix
Extraction Type
T981958
M23-I-4
ng
04/03/98
04/18/98
T
M23
Soxhlet
T981959
M23-O-1
ng
04/03/98
04/18/98
T
M23
Soxhlet
Internal Standards Percent Recovery Summary (% Rec)
13C12-^PeCDF 123 63.2 25.6 V
13C12-PeCDD 123 69.5
13C12-HXCDF 678 72.2
13C12-HxCDD 678 70.5
13C12-HpCDF 678 65.5
13C12-HpCDD 678 68.4
13C12-OCDD 40.3
31.3
35.4
36.3
33.7
38.7
25.1
V
V
V
T981960
M23-O-2
ng
04/03/98
04/18/98
T
M23
Soxhlet
54.4
62.6
74.0
71.9
67.7
77.0
47.7
Page 4
04/21/98
S982305
M23-0-3
ng
04/03/98
04/18/98
S
M23
Soxhlet
55.4
59.7
63.9
72.6
54.3
65.5
63.1
Triangle Laboratories, Inc.® Analytical Services Division
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Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 11:23 04/21/98
-------
TRIANGLE LABORATORIES OF RTF, INC. Page 5
Sample Result Summary for Project 45399 04/21/98
Method MIT2 Analysis (DB-5)
= === = = = = = = = = =============== ==== ============== === ==== ========= = = = = = = = = ===z======
Data File S982306 S982307 S982308 S982309
Sample ID M23-O-4 M23-FB-1 M23-FB-2 M23-FB-3
Units ng ng ng _ ng
Extraction Date 04/03/98 04/03/98 04/03/98 04/03/98
Analysis Date 04/18/98 04/18/98 04/18/98 04/18/98
Instrument S S S S
Matrix M23 M23 M23 M23
Extraction Type Soxhlet Soxhlet Soxhlet Soxhlet
Analytes
2378-TCDD (0.004) (0.003) (0.004) (0.003)
12378-PeCDD (0.006) (0.005) (0.005) (0.005)
123478-HxCDD (0.008) (0.005) (0.006) (0.005)
123678-HxCDD (0.007) (0.005) (0.006) (0.005)
123789-HxCDD (0.007) (0.004) (0.006) (0.005)
1234678-HpCDD {0.01} J (0.005) (0.006) (0.006)
OCDD 0.05 JB (0.006) (0.009) (0.008)
2378-TCDF 0.02 JB (0.002) 0.005 JB (0.002)
12378-PeCDF (0.004) (0.004) (0.004) (0.004)
23478-PeCDF (0.004) (0.004) (0.004) (0.004)
123478-HxCDF (0.005) (0.003) (0.004) (0.004)
123678-HxCDF (0.005) (0.003) (0.004) (0.003)
234678-HxCDF (0.006) (0.004) (0.004) (0.004)
123789-HxCDF (0.006) (0.004) (0.004) (0.004)
1234678-HpCDF (0.007) (0.004) (0.005) (0.005)
1234789-HpCDF (0.01) (0.005) (0.006) (0.006)
OCDF (0.01) (0.004) (0.006) (0.006)
TOTAL TCDD (0.004) (0.003) (0.004) (0.003)
TOTAL PeCDD (0.006) (0.005) (0.005) (0.005)
TOTAL HxCDD {0.009} (0.005) (0.006) (0.005)
TOTAL HpCDD {0.01} (0.005) (0.006) (0.006)
TOTAL TCDF 0.17 (0.002) 0.005 (0.002)
TOTAL PeCDF 0.01 (0.004) (0.004) (0.004)
TOTAL HxCDF 0.008 (0.004) (0.004) (0.004)
TOTAL HpCDF (0.008) (0.005) (0.005) 0.008
Other Standards Percent Recovery Summary (% Rec)
37C1-TCDD 91.8 93.5 92.1 93.8
Other Standards Percent Recovery Summary (% Rec)
13C12-PeCDF 234 89.7 106 107 99.6
13C12-HXCDF 478 93.4 90.4 84.6 83.7
13C12-HXCDD 478 83.8 92.9 85.0 90.3
13C12-HpCDF 789 104 110 82.6 85.4
Other Standards Percent Recovery Summary (% Rec)
13C12-HXCDF 789 87.0 84.9 85.6 88.0
13C12-HXCDF 234 86.1 87.4 87.6 87.6
Internal Standards Percent Recovery Summary (% Rec)
13C12-2378-TCDF 79.7 74.4 70.4 63.8
13C12-2378-TCDD 64.1 63.1 66.2 63.4
Triangle Laboratories, Inc.® Analytical Services Division
801 Caprtola Drive • Durham, North Carolina 27713 Printed-11 -23 04/21/98
Phone: (919) 544-5729 • Fax: (919) 544-5491 AO
-------
TRIANGLE LABORATORIES OF RTF, INC.
Sample Result Summary for Project 45399
Method MIT2 Analysis (DB-5)
Data File
Sample ID
Units
Extraction Date
Analysis Date
Instrument
Matrix
Extraction Type
S982306
M23-0-4
ng
04/03/98
04/18/98
S
M23
Soxhlet
S982307
M23-FB-1
ng
04/03/98
04/18/98
S
M23
Soxhlet
S982308
M23-FB-2
ng
04/03/98
04/18/98
S
M23
Soxhlet
Page 6
04/21/98
S982309
M23-FB-3
ng
04/03/98
04/18/98
S
M23
Soxhlet
Internal Standards Percent Recovery Summary (% Rec)
13C12-rPeCDF 123 70.7
13C12-PeCDD 123 68.3
13C12-HxCDF 678 80.5
13C12-HxCDD 678 95.3
13C12-HpCDF 678 74.4
13C12-HpCDD 678 87.2
13C12-OCDD 93.8
,1
,6
70.
83
72.8
91.7
80.5
106
119
72.
95.
96.
104
102
133
114
64.2
74.3
84.5
97.8
82.6
99.2
104
Triangle Laboratories, Inc.® Analytical Services Division
801 Capitals Drive • Durham, North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 11:23 04/21/98
43
-------
Data File
Sample ID
Units
Extraction Date
Analysis Date
Instrument
Matrix
Extraction Type
================
Analytes
2378-TCDD
12378-PeCDD
123478-HxCDD
123678-HxCDD
123789-HxCDD
1234678-HpCDD
OCDD
2378-TCDF
12378-PeCDF
23478-PeCDF
123478-HxCDF
123678-HxCDF
234678-HxCDF
123789-HxCDF
1234678-HpCDF
1234789-HpCDF
OCDF
TOTAL TCDD
TOTAL PeCDD
TOTAL HxCDD
TOTAL HpCDD
TOTAL TCDF
TOTAL PeCDF
TOTAL HxCDF
TOTAL HpCDF
TRIANGLE LABORATORIES OF RTF, INC.
Sample Result Summary for Project 45399
Method MIT2 Analysis (DB-5)
5=55 = = = = = = = = = = == = = = = === = = === = = = = = = = = = = = = = =
S982310
M23-RB-1-4
ng
04/03/98
04/18/98
S
M23
Soxhlet
(0.003)
(0.004)
(0.004)
(0.004)
(0.004)
(0.004)
(0.005)
(0.002)
(0.003)
(0.003)
(0.003)
(0.003)
(0.003)
(0.003)
(0.003)
(0.004)
(0.004)
(0.003)
(0.004)
(0.004)
(0.004)
(0.002)
(0.003)
(0.003)
(0.004)
Page 7
04/21/98
Other Standards Percent Recovery Summary (% Rec)
37C1-TCDD 83.8
Other Standards Percent Recovery Summary (% Rec)
13C12-PeCDF 234 101
13C12-HXCDF 478 82.5
13C12-HXCDD 478 82.5
13C12-HpCDF 789 95.2
Other Standards Percent Recovery Summary (% Rec)
13C12-HXCDF 789 87.7
13C12-HxCDF 234 89.1
Internal Standards Percent Recovery Summary (% Rec)
13C12-2378-TCDF 66.0
13C12-2378-TCDD 59.9
Triangle Laboratories, Inc.® Analytical Services Division
801 Capitate Drive • Durham, North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 11:23 04/21/9
-------
TRIANGLE LABORATORIES OF RTF, INC. Page 8
Sample Result Summary for Project 45399 _ 04/21/98
Method MIT2 Analysis (DB-5)
Data File S982310
Sample ID M23-RB-1-4
Units ng
Extraction Date 04/03/98
Analysis Date 04/18/98
Instrument S
Matrix M23
Extraction Type Soxhlet
Internal Standards Percent Recovery Summary (% Rec)
13C12-PeCDF 123 62.5
13012-PeCDD 123 76.1
13C12-HXCDF 678 81.6
13C12-HxCDD 678 97.6
13C12-HpCDF 678 82.8
13C12-HpCDD 678 101
13C12-OCDD 115
(Estimated Maximum Possible Concentration}, (Detection Limit) .
Triangle Laboratories, Inc.® Analytical Services Division
801 Capitals Drive • Durham, North Carolina 27713 Printed: 11 -23 04/21/98
Phone: (919) 544-5729 • Fax: (919) 544-5491
-------
TRIANGLE LABORATORIES, INC. Page 1
Sample Result Summary for Project 45399 04/20/98
Method 23X (DB-225)
sBBBBBBBBBSBBSBBBssBsssBSBSBSBBBBBBBBBBSBBBSBSBSBBSBBBBBssssssBSBSBSBBBBSBBBsssBSBS!
Data File P981305 P981306 P981307 P981308
Sample ID TLI M23 Blank M23-I-1 M23-I-2 M23-I-3
Units ng ng ng ng
Extraction Date 04/03/98 04/03/98 04/03/98 04/03/98
Analysis Date 04/16/98 04/16/98 04/16/98 04/16/98
Instrument P P P P
Matrix XAD M23 M23 M23
Extraction Type
= = = = = ===== = ==== = ==== ==== === = = = ==================== = = ========= ====== ====== ===:=====:
Analytes
2378-TCDF (0.005) {0.007}JB 0.51 {0.007}JB
Internal Standards Percent Recovery Summary {% Rec)
13C12-2378-TCDF 69.2 80.4 73.5 79.7
Triangle Laboratories, Inc.® Analytical Services Division
801 Capitola Drive • Durham, North Carolina 27713 Printed: 21:38 04/20798
Phone: (919) 544-5729 • Fax: (919) 544-5491
-------
TRIANGLE LABORATORIES, INC.
Sample Result Summary for Project 45399
Method 23X (DB-225)
Data File
Sample ID
Units
Extraction Date
Analysis Date
Instrument
Matrix
Extraction Type
==================================================:
Analytes
2378-TCDF
P981309
M23-I-4
ng
04/03/98
04/16/98
P
M23
P981310
M23-O-1
ng
04/03/98
04/16/98
P
M23
0.14
(0.01)
P981311
M23-O-2
ng
04/03/98
04/16/98
P
M23
Internal Standards Percent Recovery Summary (% Rec)
13C12-2378-TCDF 56.1 21.4 V
0.01 JB
54.0
Page 2
04/20/98
SSSSSSSSSB:
P981312
M23-0-3
ng
04/03/98
04/16/98
P
M23
(0.007)
60.0
Triangle Laboratories, Inc.® Analytical Services Division
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Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 21:38 04/20/98
-------
TRIANGLE LABORATORIES, INC. Page 3
Sample Result Summary for Project 45399 04/20/98
Method 23X (DB-225)
Data File P981317 P981319
Sample ID M23-0-4 M23-FB-2
Units ng ng
Extraction Date 04/03/98 04/03/98
Analysis Date 04/17/98 04/17/98
Instrument P P
Matrix M23 M23
Extraction Type
Analytes
2378-TCDF (0.005) (0.005)
Internal Standards Percent Recovery Summary (% Rec)
13C12-2378-TCDF 75.5 73.7
{Estimated Maximum Possible Concentration}, (Detection Limit).
Triangle Laboratories, Inc.® Analytical Services Division
801 Caprtola Drive • Durham, North Carolina 27713 Printed: 21:38 04/20/9!
Phone: (919) 544-5729 • Fax: (919) 544-5491
-------
Method 8290 Sample Calculations:
Analyte Concentration
The concentration or amount of any analyte is calculated using the following expression.
Where:
*w
C(0) = concentration or amount of a given analyte
AO = integrated current for the characteristic ions of the analyte
Ap = integrated current of the characteristic ions of the corresponding
internal standard
Qp = amount of internal standard added to the sample before extraction
RRF(0) = mean analyte relative response factor from the initial calibration
W = sample weight or volume
Detection Limits
The detection limit reported for a target analyte that is not detected or presents an analyte
response that is less than 2.5 times the background level is calculated by using the
following expression. The area of the analyte is replaced by the noise level measured in a
region of the chromatogram clear of genuine GC signals multiplied by an empirically
determined factor. The detection limits represent the maximum possible concentration of
a target analyte that could be present without being detected.
2*2.5*(F*H)*Qt
Where:
DL(0) ;
2.5
F
H
Ap
QP
RRF(0)
W
*W
estimated detection limit for a target analyte
minimum response required for a GC signal
an empirical number mat approximates the area to height ratio for a
GC signal. (F = 3.7 for all dioxin/furan analyses)
height of the noise
integrated current of the characteristic ions of the corresponding
internal standard
amount of internal standard added to the sample before extraction
mean analyte relative response factor from the initial calibration
sample weight or volume
Rev.il/19/97
49
-------
Data Flags
In order to assist with data interpretation, data qualifier flags are used on the final reports.
Please note that all data qualifier flags are subjective and are applied as consistently as
possible. Each flag has been reviewed by two independent Chemists and the impact of the
data qualifier flag on the quality of the data discussed above. The most commonly used
flags are:
A 'B* flag is used to indicate that an analyte has been detected in the laboratory method
blank as well as in an associated field sample. The 'B' flag is used only when the
concentration of analyte found in the sample is less than 20 times that found in the
associated blank. This flag denotes possible contribution of background laboratory
contamination to the concentration or amount of that analyte detected in the field sample.
An 'E' flag is used to indicate a concentration based on an analyte to internal standard
ratio which exceeds the range of the calibration curve. Values which are outside the
calibration curve are estimates only.
An 'I' flag is used to indicate labeled standards have been interfered with on the GC
column by coeluting, interferent peaks. The interference may have caused the standard's
area to be overestimated. All quantitations relative to this standard, therefore, may be
underestimated.
A * J* flag is used to indicate a concentration based on an analyte to internal standard ratio
which is below the calibration curve. Values which are outside the calibration curve are
estimates only.
A 'PR' flag is used to indicate that a GC peak is poorly resolved. This resolution problem
may be seen as two closely eluting peaks without a reasonable valley between the peak
tops, overly broad peaks, or peaks whose shapes vary greatly from a normal distribution.
The concentrations or amounts reported for such peaks are most likely overestimated.
A 'Q' flag is used to indicate the presence of QC ion instabilities caused by quantitative
interferences.
An 'RO' flag is used to indicate that a labeled standard has an ion abundance ratio that is
outside of the acceptable QC limits, most likely due to a coeluting interference. This may
have caused the percent recovery of the standard to be overestimated. All quantitations
versus this standard, therefore, may be underestimated.
An'S' flag indicates that the response of a specific PCDD/PCDF isomer has exceeded the
normal dynamic range of the mass spectrometer detection system. The corresponding
signal is saturated and the reported analyte concentration is a 'minimum estimate*. When
the 'S' qualifier is used in the reporting of 'totals', there is saturation of one (not
Data Flags Page 1 of 2
Rev. 11/19/97
-------
necessarily from a specific isomer) or more saturated signals for a given class of
compounds.
A 'U' flag is used to indicate that a specific isomer cannot be resolved from a large, co-
eluting interferent GC peak. The specific isomer is reported as not detected as a valid
concentration cannot be determined. The calculated detection limit, therefore, should be
considered an underestimated value.
A ' V flag is used to indicate that, although the percent recovery of a labeled standard may
be below a specific QC limit, the signal-to-noise ratio of the peak is greater than ten-to-
one. The standard is considered reliably quantifiable. All quantitations derived from the
standard are considered valid as well.
An 'X' flag is used to indicate that a pentachlorodibenzofuran (PCDF) peak has eluted at
the same time as the associated diphenyl ether (DPE) and that the DPE peak intensity is at
least ten percent of the total PCDF peak intensity. Total PCDF values are flagged 'X' if
the total DPE contribution to the total PCDF value is greater than ten percent. All PCDF
peaks that are significantly influenced by the presence of DPE peaks are either reported as
"estimated maximum possible concentration (EMPQ values without regard to the isotopic
abundance ratio, or are included in the detection limit value depending on the analytical
method.
DataFlags P»ge2of2
Rev. 11/19/97
51
-------
Method 23 Sample Calculations:
Analyte Concentration
The concentration or amount of any analyte is calculated using the following expression.
W
Where:
Amt<0) = amount of a given analyte, expressed in nanograms (ng) or picograms
(Pg).
Ao = integrated current for the characteristic ions of the analyte
Ap = integrated current of the characteristic ions of the corresponding
internal standard
Qp = amount of internal standard added to the sample before extraction
RRF(0) = mean analyte relative response factor from the initial calibration
W = sample weight or volume (W = 1.0 for Method 23 samples)
Detection Limits
The detection limit reported for a target analyte that is not detected or presents an analyte
response that is less than 2.5 times the background level is calculated by using the
following expression. The area of the analyte is replaced by the noise level measured in a
region of the chromatogram clear of genuine GC signals multiplied by an empirically
determined factor. The detection limits represent the maximum possible concentration of
a target analyte that could be present without being detected.
2*2.5*(F*#;*<2f»
Where:
DL(0) :
2.5 :
F
H
Ap
QP
RRFlo)
W
*w
estimated detection limit for a target analyte, expressed in ng or pg
minimum response required for a GC signal
an empirical number that approximates the area to height ratio for a
GC signal. (F = 3.7 for all dioxin/furan analyses)
height of the noise
integrated current of the characteristic ions of the corresponding
internal standard
amount of internal standard added to the sample before extraction
mean analyte relative response factor from the initial calibration
sample weight or volume
Rev. 11/19/97
-------
TLI Project: 45399
Client Sample: TLI M23 Blank
Method 23 PCDD/PCDF Analysis (a)
Analysis File: U980780
Client Project:
Sample Matrix:
TLI ID:
Sample Size:
Dry Weight:
GC Column:
r012.002/Lime Kiln
XAD
TLI Blank
i-ooo
n/a
DB-5
Date Received:
Date Extracted:
Date Analyzed:
Dilution Factor:
Blank File:
Analyst:
II
04/03/98
04/15/98
n/a
U980780
ML
Spike File:
ICal:
ConCal:
% Moisture:
% Lipid:
% Solids:
SPMIT204
UF51058
U980771
n/a
n/a
n/a
Anafytes v , -
2,3,7,8-TCDD
1,2,3,7,8-PeCDD
U,3,4,7,8.-HxCDD
U,3,6,7,8-HxCDD
1,2,3,7,8,9-HxCDD
1,2,3,4,6,7,8-HpCDD
1,2,3,4,6,7,8,9-OCDD
2,3,7,8-TCDF
1,2,3,7,8-PeCDF
2,3,4,7,8-PeCDF
1,2,3,4,7,8-HxCDF
1,2,3,6,7,8-HxCDF
2,3,4,6,7,8-HxCDF
1,2,3,7,8,9-HxCDF
1,2,3,4,6,7,8-HpCDF
1,2,3,4,7,8,9-HpCDF
1,2,3,4,6,7,8,9-OCDF
Totate
Total TCDD
Total PeCDD
Total HxCDD
Total HpCDD
Total TCDF
Total PeCDF
Total HxCDF
Total HpCDF
"'' ^ /;sPM#tffc
ND
ND
ND
ND
ND
ND
0.01
EMPC
ND
ND
ND --
ND
ND
ND
ND
ND
ND
Atnt (hj
ND
ND
- ND
ND
EMPC
ND
ND
ND
L.C-* '
0.002
0.002
0.003
0.002
0.002
0.003
0.86 38:23 J_
0.004 J_
0.002
0.002
0.002
0.002
0.002
0.002
0.002
0.002
0.003
£ \:|fciiaber> Qt ;EM^'';^w^?Sr^^|i^4^pft^);:
0.002
0.002
0.002
0.003
0.004
0.002
0.002
0.002
Page 1 of2
MTT2_PSR *UM. LARS 6.11M
Triangle Laboratories, Inc.*
801 Capitola Drive • Durham, North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 13:40 04/20/98
53
-------
TLI Project:
Client Sample:
45399
TLI M23 Blank
Method 23 PCDD/PCDF Analysis (a)
Analysis File: U980780
'3C,r2,3,7,8-TCDF
'3CI2-2,3,7,8-TCDD
13C,2-l,2,3,7,8-PeCDF
13C,:-l,2,3,7,8-PeCDD
'3C,2-l,23,6,7,8-HxCDF
13C,2-l,2,3,6,7,8-HxCDD
13C,:-l,2,3,4,6,7,8-HpCDF
'3C,:-l,2,3,4,6,7,8-HpCDD
I3C,:-1,2,3A6,7,8,9-OCDD
2.6
2.7
2.7
4.0
2.7
3.1
3.3
3.7
6.6
65.8
67.9
68.6
99.4
68.1
78.7
83.7
92.5
83.0
40%-130%
40%-130%
40%-130%
40%-130%
40%-130%
40%-130%
25%-130%
25%-130%
25%-130%
0.77
0.81
1.48
1.50
0.50
1.23
0.39
1.00
0.87
23:21
24:07
27:32
28:38
31:15
31:57
34:04
35:03
38:22
Surrogate Standards {Type A)
13C,2-2,3,4,7,8-PeCDF
l3C.2-l,2,3,4,7,8-HxCDF
13C,2-l,2,3,4,7,8-HxCDD
IJCis-lA3A7,8,9-HpCDF
4.2
4.3
4.6
3.6
106
108
114
90.1
40%-130%
40%-130%
40%-130%
25%-130%
1.46
0.49
1.22
0.42
28:17
31:10
31:53
35:30
Other Standard
Amt,
"CU-WJ.S-TCDD
3.5
87.9
40%- 130%
24:08
Alternate Standards (Type A) Amt. (ngj
'3C,2-l,2,3,7,8,9-HxCDF
13Cl2-2,3,4,6,7,8-HxCDF
3.4
3.3
84.5
81.8
40%-130%
40%-130%
0.50
0.50
32:30
31:46
Recovery Standards
13C12-1,2,3,4-TCDD
13C12-l,2,3,7,8,9-HxCDD
0.82
1.20
23:55
Data Reviewer
Page 2 of2
04/20/98
Mrnj>SRvl.04, LARS 6.11.00
Triangle Laboratories, Inc.*
801 Capitola Drive • Durham, North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 13:40 04/20/98
-------
Initial
Dae*..
Data Review By:
Calculated Noise Area:
4.07
The Total Area for each peak with an ion abundance ratio outside
ratio limits has been recalculated according to method requirements.
Page No.
04/20/98
Listing Of 0980780B.dbf
Hatched GC Peaks / Ratio / Ret. Time
Compound/
M_Z QC.Log Omit Why . .RT. OK Ratio Total.Area... Area.Peak.1.. Area.Peak.2.. Rel.RT Compound.Dame.. ID.. Flags.
TCDF
304-306
304-306
0.65-0.89
DC NL 0:00 RO 0.62 15.06
23:22 RO 0.45 32.25
1 Peak 32.25
14.03
0.844-1.086
0.000
31.51 1.001 2378-TCDF
AH J
13C12-TCDF
316-318
316-318
TCDD
320-322
320-322
37C1-TCDD
328
328
13C12-TCDD
332-334
332-334
PeCDF
340-342
0.65-0.89
DC
DC
NL 0:00
WL 22:
13
RO
22:54
23:
23:
21
49
RO
1.
0.
0.
0.
0.
96
76
87
77
99
3 Peaks
DC
DC
D
DC
DC
NL 0:
SN 23:
SN 24:
00
20
08
SN 24:21
SN 24:
30
0.
RO
RO
RO
RO
RO
65-0.89
0.
3.
0.
1
1
.63
.39
.43
.36
.70
0 Peaks
DC
NL 0:00
22:
:37
24:08
2 Peaks
DC
NL 0:00
22
23
24
24
:53
:55
:07
:29
0.
RO
RO
65-0.
2
1
0
0
0
.10
.12
.82
.81
.79
89
4 Peaks
DC
DC
DC
NL 0
SN 25
SN 25
:00
:29
-.48
1,
RO
RO
RO
.32-1.
0
2
0
1 AJ
78
.84
.89
.72
6.21
318.34
121.02
27,052.70
69.14
27,242.86
/
4.90
8.18
18.35
2.60
2.16
0.00
1.39
17.02
18,717.10
18,734.12
13.54
104.54
28,009.20
21.268.95
318.23
49,700.92
Above:
DC SN 26:05 RO 0.47
4.33
5.38
3.36
3.64
56.22
11,732.50
38.57
Follows
17.02
18.717.10
66.07
12.615.40
9,538.45
140.18
Follows
0.957-1.043
0.000
0.951
64.80 0.981
15,320.20 1.000 13C12-2378-TCDF ISO
39.06 1.020
0.878-1.050
0.000
0.968
1.001 2378-TCDD
1.010
1.016
0.917-1.083
0.000
0.938
1.001 37C1-TCDD
AN
CLS
0.917-1.083
0.000
59.06 0.949
15,393.80 0.992 13C12-1234-TCDD RSI
11,730.50 1.000 13C12-2378-TCDD 1S1
178.05 1.015
0.917-1.068
0.000
0.926
0.937
0.947
Triangle Laboratories, Inc.® Analytical Services Division
801 Capftola Drive • Durham, North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 13:4004/20/98
55
-------
Page No.
04/20/98
Listing of U980780B.dbf
Matched GC Peaks / Ratio
/ R«t. HIM
Coqpound/
M_Z ____ QC.Log Omit Why . .RT. OK Ratio Total . Area ... Area. Peak. 1 .. Area. Peak. 2. . Rel.RT Coapound.NUM.
ID.. Flags.
340-342
13C12-PeCDF
352-354
352-354
PeCDD
356-358
356-358
13C12-PeCDD
368-370
368-370
HxCDF
374-376
DC SN 26:26 RO
DC SN 26:39 RO
DC SN 26:49
DC SN 26:58 RO
DC SN 27:10 RO
DC SN 28:11
DC SN 28:17 RO
DC SN 28:25
DC SN 29:14 RO
DC SN 29:20 RO
0 Peaks
1.:
DC NL 0:00
26:38
27:10
27:32
27:51
28:17
28:38
29:16
7 Peaks
1.
DC NL 0:00 RO
DC SN 26:55 RO
D SN 27:32 RO
DC SN 27:39
D SN 28:17
DC SN 28:36 RO
DC SN 29:05 RO
DC WH 29:22 RO
DC WH 29:38 RO
0 Peaks
1.
DC NL 0:00 RO
27:32
28:38
28:46
29:00 RO
4 Peaks
1
DC NL 0:00
DC SN 31:11
DC SN 31:53 RO
DC SN 31:56 RO
0.16
0.57
1.43
0.43
0.52
1.73
2.08
1.50
0.99
0.72
12-1.78
1.46
1.49
1.34
1.48 21,
1.53
1.46 22,
1.66
1.58
45,
— — — — &>v%va * C
32-1.78
0.69
0.59
1.08
1.72
1.77
2.08
0.93
0.36
1.17
32-1.78
0.98
1.64
1.50 16
1.53 1
3.03
17
.05-1.43
1.30
1.07
0.71
0.25
1.07
5.74
1.65
2.50
5.91
4.61
5.99
4.95
4.95
2.50
0.00
3.27
515.16 308.00
43.38 24.88
926.89 13,102.30
168.38 101.84
359.52 13,285.30
44.32 27.66
65.71 40.27
123.36
>*»f*T\J? / PaT*nn T?rtl 1 nwa - — •
'V*~Uf I FV^~W f OiAOWS •*
1.83
5.26
15.14
3.13
15.90
3.70
4.28
2.37
6.70
0.00
2.39
28.72 17.85
,427.29 9,847.36
,424.21 860.99
13.36 15.88
,893.58
Dafnn / UvfTM? TPrtl 1 /M*r« <•»-
jre<_uu / nxv~Lv e o A .LOWS -•
10.44
8.09
4.15
3.16
0.960
0.968
0.974
0.979
0.987
1.024
1.027 23478-PeCDF
1.032
1.062
1.065
0.855-1.145
0.000
207.16 0.967
18.50 0.987
8,824.59 1.000 13C12-PeCDF 123
66.54 1.012
9,074.22 1.027 13C12-PeCDF 234
16.66 1.040
25.44 1.063
0.928-1.022
0.000
0.940
0.362
0.96d
0.988
0.999 12378-PeCDD
1.016
1.026
1.035
0.860-1.140
0.000
10.87 0.962
6,579.93 1.000 13C12-PeCDD 12:
563.22 1.005
5.24 1.013
0.959-1.047
0.000
0.998 123478-HXCDF
1.020
1.022
AN
IS2
SUR1
AN
> IS3
AN
Triangle Laboratories, Inc.® Analytical Services Division
801 Caphola Drive • Durham, North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 13:40 04/2019
-------
Page No. 3
04/20/98
Compound/
M_Z QC.Log Omit Why
Listing of 0980780B.dbf
Matched GC Peaks / Ratio
/ Ret. Time
.RT.
OK Ratio Total.Area... Area.Peak.1.. Area.Peak.2.. Rel.RT Conpound.Nane.. ID.. Flagi
D
374-376
13C12-HXCDF
384-386
334-386
HXCDD
390-392
D
D
390-392
i3c 12 -HXCDD
402-404
402-404
HpCDF
408-410
408-410
13C 12 -HpCDF
418-420
418-420
DC SN 32:04 RO 0.34
DC SN 32:07 RO 2.02
DC SN 32:11 RO 3.67
DC SN 32:29 RO 0.73
D SN 32:31 1.11
DC WH 32:55 RO 0.42
0 Peaks
0.43-0.59
DC NL 0:00 RO 1.27
30:10 0.45
30:18 0.47
31:10 0.49
31:15 0.50
31:46 0.50
32:30 0.50
1.64
2.93
2.53
6.20
11.58
3.54
0.00
11.01
211.83 66.19
252.65 80.95
19,894.83 6.563.63
22,345.35 7,415.55
24,229.50 8,099.80
19,282.44 6,456.14
1.026
1.028
1.030
1.039 123789-HxCDF AH
1.041
1.0S3
0.872-1.128
0.000
145.64 0.965
171.70 0.970
13,331.20 0.997 13C12-HXCDF 478 SUR2
14,929.80 1.000 13C12-HXCDF 678 IS4
16,129.70 1.017 13C12-HXCDF 234 ALT2
12,826.30 1.040 13C12-HXCDF 789 ALT1
6 Peaks 86,216.60
1.05-1.43
DC NL 0:00 RO 0.83
D SN 31:10 RO 1.95
D SN 31:16 RO 2.30
DC SN 31:47 RO 3.01
DC WH 32:30 RO 8.36
0 Peaks
1.05-1.43
DC NL 0:00 RO 1.03
31:22 1.17
31:53 1.22
31:57 1.23
32:16 1.20
9.45
13.75
13.53
9.61
4.75
0.00
15.99
76.16 40.99
15,985.15 8,798.58
19,092.35 10,538.10
24,384.70 13,317.20
0.955-1.014
0.000
0.975
0.979
0.995
1.017
0.969-1.031
0.000
35.17 0.982
7,186.57 0.998 13CI2-HXCDD 478 SOR3
8,554.25 1.000 13C12-HXCDD 678 IS5
11,067.50 1.010 13C12-HXCDD 789 RS2
4 Peaks 59,538.36
0.88-1.20
DC NL 0:00 RO 2.42
DC SN 34:06 RO 2.70
DC SN 35:27 1.08
DC SN 35:36 RO 3.00
DC WH 35:43 RO 2.77
0 Peaks
0.37-0.51
DC NL 0:00 RO 0.60
34:04 0.39
35:30 0.42
2 Peaks
4.92
6.94
3.32
4.75
3.53
0.00
9.13
16,774.71 4,735.81
12,127.45 3,608.54
28.902.16
0.995-1.047
0.000
1.001 1234678-HpCDF AN
1.041
1.045
1.048
0.941-1.117
0.000
12,038.90 1.000 13C12-HpCDF 678 IS6
8,518.91 1.042 13C12-HpCDF 789 SUR4
Triangle Laboratories, Inc.® Analytical Services Division
801 Caprtola Drive • Durham, North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 13:40 04/2088
57
-------
Page No.
04/20/98
Lilting of T)980780B.dbfi
Matched <3C Peaks / Ratio
/ Ret. Tin*
Compound/
M_Z QC.Log Omit Why . .RT. OK Ratio Total.Area... Area.Peak. 1. . Area.Peak.2.. Rel.RT Compound.Name.. ID.. Flags.
Above: HpCDF I HpCDD Follows
HpCDD
424-426
424-426
13C12-HPCDD
436-438
436-438
OCDF
442-444
0.88-1.20
DC NL 0:00 RO 0.36 1.61
DC WL 34:03 RO 2.59 10.38
DC SN 34:38 RO 4.74 2.33
0 Peaks 0.00
0.88-1.20
DC NL 0:00 RO 1.38 13.63
34:21 RO 1.30 80.62
35:03 1.00 16,382.49
2 Peaks 16,463.11
51.37
8,187.87
0.975-1.005
0.000
0.971
0.988
0.971-1.029
0.000
39.52 0.980
8,194.62 1.000 13C12-HpCDD 678 IS7
442-444
0.76-1.02
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
NL
SN
SN
SN
SN
SN
SN
SN
SN
SN
SN
SN
1
0:00
34:34
34:39
35:03
35:29
35:37
35:48
35:54
36:54
38:51
40:39
40:46
40:55
Peak
RO
RO
RO
RO
RO
RO
RO
RO
RO
RO
RO
RO
0.
1.
0.
1.
1.
1.
1.
0.
2.
0.
2.
1.
1.
97
05
72
89
15
35
10
63
02
35
08
91
,18
Above: HpCDD / Octa-CDD and CDF Follows
0.896-1.104
4.97 0.000
1.78 0.901
4.16 0.903
10.05 10.07 5.32 0.914
6.41 0.925
3.74 0.928
4.16 0.933
6.99 0.936
3.59 0.962
1.34 1-013
1.49 1.060
1.08 1.063
2.91 1.066
10.05
OCDD
458-460
458-460
0.76-1.02
DC NL 0:00 RO 2.18
38:23 0.86
1 Peak
2.10
37.20
37.20
17.20
0.896-1.104
0.000
20.00 1.000 OCDD
13C12-OCDD 0.76-1.02
470-472 DC NL 0:00 RO 2.50 1.91
38:22 0.87 22,056.70
470-472 1 Peak 22,056.70
10,248.60
0.995-1.004
0.000
11,808.10 1.000 13C12-OCDD
IS8
Column Description.
H_Z -Nominal Ion Mass(es)
"Why" Code Description QC Log Desc.
WL-Below Retention Time Window A-Peak Added
. .RT. -Retention Time (mn:ss) WH-Above Retention Time Window K-Peak Kept
Rat.l -Ratio of M/M+2 ions
OK -RO»Ratio Outside Limits
Rel.RT-Relative Retention Time
End of Report
SN-Below Signal to Noise Level
-------
riles 09 807 80 §1-893 AcqslS-APS-1998 20:48:51 CC EH- Voltage SIS 70S Noimei3276
303.9016 Ft2 BSUB(256,30,-3.0) PKD(9, 5,3, 0.10\,13104 .0, 1.00\,r,T) XxptXDBSOS
TRIANGLE LABS Text: HI H23 BLANK TLH45399
1001 A1.4025 3.524
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60:
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0:
AS. 26X4 || I I
1 1 A3. 89X4 M l\ L I i .
.2.814
.2.124
.1.424
.7.123
.0.020
'ao'iOO ' ' ' '21:00 ' ' ' '22:00' ' ' ' '.2.3:00 24:00 25:00' ' Time
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305.8987 F:2 BSUB(256,30, -3 .0 ) PKD(9,5 ,3,0 .10\,20984 .0,1.00\,T,T) ExpsNDBSOS
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100* A3. 5E5 C8.3E4
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315.
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330.
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9419 F:2 BSUB(256,30, -3.0) PKD(9,5,3, 0.101,13764 .0,1 . 00%,f, T) Exp:NDB5US
NGLE LABS T«It:TEI M23 BLANK TLIf 45399
A1.17E8
11
20:00 21:00. 22:00 23:00 24:00 25:00
: 0980780 #1-893 Acq:15-APS-1998 20:48:51 GC EI+ Voltage SIR 70S Noise: 1753
9389 Fs2 BSUB(256,30,-3.0) PKD(9 ,5,3,0. 10\,7012. 0,1. 00\,r,T) ExpsNDBSUS
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Al . 53E8
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11
20:00 21:00 22:00 23:00 24:00 25:00
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20:00 21:00 22:00 23:00 ' '24:00 ' '25ioo'
.10980780 #1-893 Aoj:15-APJ?-199fl 20:48:51 CC EH- Voltage SIR 70S
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•^-^W^M^fJ^^
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20 100 21 100 22:00 23:00 24:00 25>00
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0.0X0
Time
.2.7X7
-.2.2X7
-.1 . 6E7
.1.1X7
.5.4X6
O.OEO
Time
-3.5E7
.2.8E7
.2.127
.1 . 427
.6.92$
0.020
rue
5.427
1.4.327
.3.227
.2.227
.1.127
.0.020
Time
-4.124
13.324
k:2.424
.l.«4
.a. 123
4.0.020
Time
-------
Tiles 0980780 tl-893 Acqil5-APX-1998 20:48:51 GC £J+ Volt*9* SIM 708 MoimmilOSS
319.8965 Fi3 3803(256,30,-3.0) tKD(7,5,3,0.10\,4260.0,1.00\,f,T) XzpsKDBStTS
TRIANGLE LABS TeJCtsTLI H33 BLANK TLH4S399
100\ _ A1.57X5
22iOO 23:00 24»00 25:00
1*110:17580700 #1-853 Acqsl5-APX-1998 20:48:51 GC XI + Voltage SIX 70S Halfet1687
321.8936 rt2 BSOS(256, 30, -3.0) PKD(7,S,3,0.10\,6748.0,1.00\,T,T) XxpsXDBSUS
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1001 . . Al.
22:00 , 23:00 24:00 25:00
Tiles0980780 tl-893 AoqilS-APR-1998 20:48:51 GC EH- Voltage SIX 70S Noiaes8036
331.9368 JT:2 BSOB(256,30, -3. 0) PKD(7,5,3,0.10\,32144.0,1.00\,T,T) XxptNDBSOS
•TRIANGLE LABS TexttTLI H23 BLANK TLIt4S399
1003
80:
60.
40.
20.
22:00 23:00 24:00 25:00
rileiO980780 tl-893 Acqsl5-APX-1998 20:48:51 GC EI+ Voltage SIX 70S Noiaes3827
333.9338 Ts2 BSOB(256,30,-3.0) PKD(7,5,3,0.10\,153Q8.0,1.00\,F,T) ExpsNDBSUS
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80;
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22:00 23:00 24:00
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327.8847 n2 BSUS(256, 30, -3, 0) PXD(7,5,3,0.10\,2784.0,1.00\,r,T) EzpsSDBSVS
TRIANGLE LABS Text:HI M23,' BLANK TLIt4S399
1001 A1.87E8
80:
60: i
40:
20:
25:00
.3.0X4
.2.4X4
.1.8X4
.1.2X4
5.9X3
0.0X0
Time
AJ.
1
/ote
54r7
\
3.0F7
2.4X7
1.8X7
1.2E7
6.0E6
O.OEO
Time
3.6E7
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2.1X7
.1.4X7
.7.2X6
0.0X0
Time
4.4X7
3. SE7
.2.6X7
Ll. 8X7
'•8.8X6
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22:00
rile:E7980780 #1-893 Aoj:15-APK-lS98
330.9792 ft 2 ExpsNDBSUS
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100\i*~j»~~ ^£iii3 JH>
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339.8597 Ti2 BSUB(256,30,-3.0) PKD(7, 5,3,0.10\, 5268.0,1.00\,F,T) Xxp:NDB5OS
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1001
sol
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A3.78S4
25:00 27:00 28:00
File:U980780 §1-893 Acqi15-APR-1998 20:48:51 GC XI+ Voltage SIS 70S Noime:1568
341.8567 T:2 BSUB(256,30, -3.0) PKD(7,5,3,0.10\,6272.0,1.00\,F,T) ExpiNDBSUS
TRIANGLE LABS TeittTLI H23 BLANK TLH45399
ion
29tOO
80:
60:
40:
20:
7X4
A6.08S4
26i00 27:00 28:00
Tile:U980780 91-893 Acq:15-APR-1998 20:48:51 GC EH- Voltage SIS 70S tfoi.ae-.971
351.9000 ri2 BSUB(256,30,-3.0) PKD(7,5,3,0.10\,3884.0,1.00\,F,T) ExpiHDBSUS
TRIANGLE LABS Text.-TLJ M23 BLANK TLIV45399
1001, A1.31S8 A1.33E8
80:
60:
40:
20:
29:00
26:00 27:00 28:00
Filesa980780 tl-893 Acq:15-APR-1998 20:48:51 GC EI+ Voltagre SIR 70S Noise:666
353.8970 F:2 BSUB(256,30, -3. 0) PKD(7,5,3, 0.10\,2664.0,1. 00\,F,T) ExpiNDBSUS
TRIANGLE LABS Text-.TLI M23 BLANK TLI#45399
1004 A8.82E7 A9.07E7
29:00
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.2.1X4
.1.6X4
-.1.1X4
.5.3X3
0.0X0
T±m»
3.8X4
3.1X4
2.3X4
.1.5X4
.7.6X3
.0.0X0
Tif
.3.8X7
.3.0X7
.2.3X7
.1. 5X7
.7.5X6
.O.OEO
Time
-2.6E7
80.
60:
40:
20:
0
Tile
330.
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1003
80:
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20^
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25:31 25:47 26:09 27:00
26.00
10980780 tl-893 Acq: 15-APR-1998 2
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Time
-6.5X4
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'.1.3X4
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Time
-------
Fij.eiuyau/uu ti-usi Acyii.3-Kex-t.999 aotiatsi ec EH- voj.t*gm SIM fas
355.8546 T>2 BSVB(256,30,-3.0) PKD(5r 5,3,0.05\,2220.0,1.00\,f,T) XxpiXDBSUS
TRIANGLE LABS TmxtiTLI M23 BLANK TLHM5399
27i00 28tOO 29t00
rila10980780 #1-093 Acq,15-APR-1998 20i48t51 GC XI+ Voltage SIX 708 Solt»t801
357.8516 Ts2 BSOB(256,30, -3.0) PKD(5, 5,3,0.05\, 3204.0,1.00\,r,T) XxpiUDBSOS
TXIABGLS LABS TextiTLI H23 BLANK TLH45399
1004 A5.40E4
80.
60.
40.
20.
27:00 28i00 29:00
TiletV980780 #1-893 Acq:15-APX-1998 20:48:51 GC EH- Voltage SIR 70S Noise-.727
367.8949 T:2 BSUB(256,30, -3. 0) PKD(5,5,3, 0.05\,2908.0,1.00\,r,T) ExpsKDBSOS
TXIASGLE LABS Teit-.TLI H23 BLANK TLI#45399
1001 A9.S5E7
so:
60.
40:
201
B.61E6
27i00 28tOO 29,00
File:D980780 #1-893 AcqslS-APX-1998 20:48:51 GC EI+ Voltage SIR 70S Noifa:740
369.8919 Ts2 BSUB(256,30, -3.0) PKD(5,5,3,0.OS\,2960.0,1.00\rr,T) ExptNDBSUS
TRIANGLE LABS Text-.TLI H23 BLANK TLI#45399
1003k A6.58E7
80.
60.
40.
20.
0.
27:00 28:00
File:O980780 tl-893 Acq:15-APR-1998 20:48:51 GC CI+ Voltage SIR 70S
330.9792 Ti2 ExpsNDBSUS
TRIANGLE LABS TcxttXLX M23 BLANK TLH45399
.63E6
29100
80.
60.
40.
20.
0.0X0
Timi
.2.4X4
'.1.9E4
-1.4E4
.9. 5E3
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Tims
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2.4E7
1.. 8E7
1.2E7
6.1E6
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Time
-2.0E7
"-1.6E7
-1.2E7
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0.0X0
Tim
.4.6X7
.3.4X7
.2.3X7
.1.1X7
27:00
28100
29100
'.0.0X0
Tim
-------
30100 30,12 30:24 30,36 30,48 31:00 31tl2 31:24 31:36 31:48 32:00 32:12 32:24 32:36 32:48 33:00
ile:O980780 tl-413 Acq,15-APX-1998 20t48tSl QC fl+ Voltage SIX 70S Koife:2272
75.8178 F,3 BSUB( 256,30,-3.0) PXD(7,5,3, 0.101,9088.0,1. 00\,F,T) Ezp:NDB5OS
TRIANGLE LABS Text:TLI H23 BLANK TLIt45399
ile:O980780 tl-413 Aoqtl5-APX-1998 20:48:51 CC SI+ Voltage SIX 70S Noise:2952
73.8208 T:3 BSUB(256,30,-3.0) PXI>(7,5,3,0.10\, 11808.0,1.00\,F,T) XxpiHDBSUS
IANGLE LABS Tej[t:TLI M23 BLANK TLIt45399
A4.19E4 A6.08X4
Time
3o':b6' 30\12 30:24 30:36 30t48 31iOO 31:12 31t24 31:36 31:48 32:00 32:12 32:24 32:36 32:48 33:00
•ile:U980780 tl-413 Acq:15-APX-199S 20:48:51 GC EH- Voltage SIX 70S Noiae:4632
83.8639 F:3 BSUB(256,30,-3.0) PKD(7,5,3, 0.101,18528. 0,1.00%,F,T) Exp:NDB5US
TRIANGLE LABS Text:TLI H23 BLANK TLI#45399
Zuie
1005
so:
60:
40:
20:
A8.10E7
A6.56E7
A6.46E7
-.2.1E7
.1.6E7
.1.1E7
.S.4E6
O.OEO
30-00 30:12 30:24 30:36 30:48 31:00 31:12 31:24 31:36 31:48 32:00 32:12 32:24 32:36 32:48 33:00
File:0980780 tl-413 Acq:15-APS-1998 20:48:51 GC EI+ Voltage SIR 70S Noiae:3646
385.8610 F:3 BSOB(256,30, -3.0) PKD(7, 5,3, 0.10%, 14584 . 0, 1. 00\,F,T) Eip:NDB5OS
TRIANGLE LABS Teit-.TLI M23 BLANK TLIt45399
Time
1001
BO:
60:
40:
20:
Al. 61E8
A1.49E8
A1.28E8
30:00 30:12 30:24 30:36 30:48 31:00 31:12 31:24 31:36 31:48 32:00 32:12 32:24 32:36
rile.-0980780 tl-413 Acg:15-APR-1998 20:48:51 GC Eli- Voltage SIR 70S
392.9760 F:3 ErpsNDBSUS
TRIANGLE LABS Teit:TLI M23 BLANK TLH45399
,.,^,-^J£j&*«j*3Sil£^^ 3a'00 32:1933,30
80^"*"
60:
40:
20:
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32:48 33:00 Tim
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L2.1E7
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30:00 30:12 30*24 30:36 30:48 31:00 31:12 31:24 31:36 31:48 32:00 32:12 32:24 32:36
Fila:U980780 tl-413 Acq:15-APX-1998 20:48:51 6C EH- Voltage SIX 70S
445.7555 F:3 Exp:NDBSUS
TRIANGLE LABS Text:TLI M23 BLANK TLH45399
\0. OEO
32':48' jjibb Tim
.2.5E7
.2.0E7
.1.5E7
-.1.0E7
1.5. OE6
30,00 30,12 30,24 36,36 30,48 31,00 31:12 31:24 31:36 31,48 32:00 32:12 32:24 32:36
O.OfO
32:48 33:00 Tim
-6.1E4
.4.9X4
-------
>il»,VSB07BO tl-413 Acq,15-Af*-lSS8 30:48,51 CC SH- Volt«y« SIS 70S lbit*,3614
89.8156 Ft3 BSUB(256,30,-3.0) PKD(7,5,3,0.10\,10456.0,1.00\,F,T) SxpttOfSUS
TRIANGLE LASS TmjcttTLI M23 BLANK TCI#45399
001 HI.39X5
80.
60.
40.
201
Al.7715
30,36 30,48 31,00 31,12 31,24 31,36 31,48 32,00 32,12 32,24
Fll*:U9807aO 11-413 Acq:15-APR-1998 20,48,51 CC EH- Voltagr. SI* 70S KOimm,3167
91.8127 T,3 BSUB(256,30,-3.0) PKD(7,5,3,0.10\,12668.0,1.00\,T,T) Exp:XDB5US
TRIANGLE LABS Text!IXJ H23 BLANK TLIf 45399
1003k A6.14X4
32,36
30t36 30:48 31,00 31:12 31:24 31,36 31,48 32,00 32,12 32:24
File:0980780 #1-413 Acq:15-APS-1998 20:48:51 GC EI+ Voltage SIX 70S Kois9:4424
401.8558 r:3 BSUB(256,30, -3.0) PJO>(7,5,3, 0.10\,17696.0,1.00\,F,T) Exp:HDBSVS
TRIANGLE LABS Text.-HI M23 BLANK TLI#45399
1004 A1.33E8
32,36
801
601
40.
20.
Al.OSES
30:36 30:48 31:00 31:12 31,24 31:36 31:48 32:00 32:12 32J24
F±le:V980780 #1-413 Ac?:15-AP£-1990 20<48>51 GC EI+ Voltage SIR 70S Noia*:4307
403.8529 F:3 BSUB(256,30,-3.0) PKD(7,5,3,0.10\,17228.0,1.00\,F,T) Ezp,NDB5OS
TRIANGLE LABS TextiTLI H23 BLANK TLI#45399
A1.11E8
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60.
40.
20.
32:36
30,36 30:48 31,00 31,12 31,24 31,36 31:48 32:00
rile:U980780 fl-413 Acq:15-APR-1998 20,48:51 GC EI+ Voltage SIR 70S
392.9760 F:3 SxpsHDBSUS
TRIANGLE LABS T«xt.-IXJ M23 BLANK TLI44S399
32:12 32:24
32,36
1003
80.
60.
40.
20.
0.
30138
30:57 31,06
31.45
4.1X4
3.3X4
2.5E4
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Time
4. 1E7
3.2E7
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O.OEO
Tin.
3.4E7
2.7E7
2.0E7
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Tim
30\36 '30',48 'Jit00' ' 3lil2 ' '31i24' ' '3l't36 ' '3l'i48 ' 32iOO ' '32:12
3.5X7
2.0X7
1.5X7
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-------
'He ,09 807 80 tJ.-662 Acqil5-APS-1998 20,48*51 GC EH- Voltage SIX 70S Hoi»ei2920
07.7818 Ti4 BSOB(256,30,-3.0) fKD(7,5,3,0.10\,11680.0,1.00\,T,T) SxptHDBSUS
TRIANGLE LABS Text: TLI M23 BLANK TLI#45399
100*
A9.19E4
34iOO 34>12 34i24 34,36 34i48 35*00 35tl2 35>24 35t36
File:U980780 #1-662 Acq:15-APS-1998 20>48i51 GC XI* Voltage BIS 70S No±fe:1203
409.7789 n4 BSOB(256,30,-3.0) PKD(7,5,3,0.10\,4812.0t1.00\,reT) Exp:NDB5US
TRIANGLE LABS Text: TLI M23 BLAHK TLI#45399
A5.88X4
80:
60.
40:
201
Al. 72X4
.4.2X4
.3.4X4
.2.5X4
.1. 7X4
.8.4X3
0.0X0
35:48
36100 Time
34:00 34:12 34:24 34:36 34,48 35:00 35:12 35,24 35:36
rile:D980780 tl-662 AcqslS-APS-1998 20:48:51 GC EI+ Voltago SIS 70S Noi*u:1898
417.8253 F:4 BSUB(256,30, -3. 0) PKD(7,5,3,0.10\, 7592. 0,1.00\,r, T) XxpsNDBSUS
TRIANGLE LABS Text.-IXI M23 BLAHK TLI#45399
100* A4.74E7
35,48
80:
60:
40:
20:
o:
A3.61E7
T
T
T
T
T
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34:00 34:12 34i24 34:36 34:48 351-00 35:12 35:24 35:36
rila:U980780 #1-662 Acq:15-APX-1998 20:48:51 GC EH- Voltage SIR 70S Noiae:3168
419.8220 T:4 BSUB<256, 30, -3. 0} PKD(7,5,3,0.10\,12672.0f1.00\rF,T) Exp:IO)B5US
TRIANGLE LABS Text:TLI H23 BLANK TLI#45399
1001
BO':
60:
40:
20:
0:
A1.20E8
A8.52E7
T
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34:00 34:12 34':24 34:36 34:48 35:00 3S':12 35:24
File:U980780 #1-662 AcqslS-APS-1998 20:48:51 GC EI+ Voltage SIS 70S
430.9729 F:4 Exp:NDB5OS
TSIANGLE LABS Text:TLI M23 BLANK TLI#45399
100* 34:05 . 34:16 . „.„ J.,,., .. „ ..... 35.36
80J
60:
40:
20:
0.
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35.-35
35\48
35:47
34:00 34:12 34:24 34:36 34:48 35:00 35:12 35:24
File,0980780 #1-662 AcqslS-APR-1998 20:48:51 GC XI+ Voltage SIS 70S
479.7165 F:4 Exp:NDB5VS
TRIANGLE LABS Text:TLI M23 BLANK TLI#45399
100* 35,05
35:36
35\48
.0X0
Time
i i | ' i i i i I
35:40 36:00
Lo.
36:00
,4X7
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.5X6
.7X6
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Time
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Time
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3E7
OE7
6E6
3X6
OEO
Time
-------
ile:U9S0780 #1-662 Acq:15-APR-1998 20:48:51 GC EH- Voltage SIX 70S Boim*>1133
25.7737 Fs4 BSVB(256,30, -3.0) PKD(7,5,3,0.10\,4532.0,1.00\,F,T) ExptODBSOS
TRIANGLE LABS TextiXLX H23 BLANK TLI#45399
A6.15E4
'He,09607BO tl-662 Acq:lS-AfX-199B 20,4B,51 GC B+ Voltay. SIS 70S Soi.»»i409
23.7766 F>4 BSUB(256,30,-3.0) fgD(7,5,3,0.10\,1636.0,1.00\,r,T) fxpiODBSUS
lAHSLE LASS TmxtsXLX M23 BLANK TLII45399
001
34tl8 34i24 34s30 34t36 34t42 34:48 34:54 35:00 35tOf 35tl2 35tlS 35124 35:30
1. 8X4
.1.5E4
O.OEO
34:12 34:18 34s24 34:30 34:36 34:42 34:48 34:54 35:00 35:06 35:12 35:18 35:24 35:30
'ile:U980780 fl-662 Acq:15-APS-1998 20:48:51 GC EH- Voltage SIX 70S Xoiee:4602
35.8169 F:4 BSUB(256,30, -3.0) PKD(7,5,3,0.101,18408.0,1.00\,r,T) ExpsNDBSaS
TRIANGLE LABS TextiZZJ H23 BLANK TLHH5399
A8.19E7 2.2E7
Tims
80.
eo:
4 a:
20.
34:12 34:18 34:24 34:30 34:36 34:42 34:48 34:54 35:00 35:06 35:12 35:18 3's\24' J5-JO
rile:U980780 il-662 Acq:15-APX-1998 20:48:51 GC EH- Voltage SIX 70S Noise:3339
437.8140 F:4 BSUB(256,30, -3.0) PKD(7,5,3,0.10\,13356. 0,1.00\,T,T) Exp:KDB5aS
TRIANGLE LABS TextilXZ M23 BLANX TLIt45399
100* A8.J.9E7
80.
601
40.
20.
,1. 8E7
1.3E7
.8.9E6
.4.5E6
.O.OEO
Tim
2.2E7
1.8E7
1.3E7
8.9E6
.4.4E6
'
34:12 34:18 34:24 34:30 34:36 34:42 34:48 34:54 35:00 35:06
File:U980780 fl-662 AcqtlS-APX-1998 20:48:51 GC EI+ Voltage, SIX 70S
430.9729 F:4 ExpiNDBSUS
TRIANGLE LABS TtocttTLI M23 BLANK TLH4S399
"°V 34>i6 --• -" ""- 34,5,
--~ - \~/^s^\/~^ .^^v^yN/v x^. _
80.
00:
40.
20.
0.
J5.' 18 ' '35-24 '
O.OEO
Tim
35 > 15
35:28
,.1.7X7
.J..3E7
.1.0X7
.6.6E6
'.3.3X6
34\12'
3424 3430 34t36
34i48' '34t54'
35112' 35': 18 ' 35>24' 35': 30
O.OEO
Tim
-------
34:00 35:00 . 36:00 37s00 38:00 39:00 40:00
File:O980780 fl-662 Acq:15-APR-1998 20:48:51 GC EI+ Voltage SIS 70S No±ae:1262
443.7399 F:4 BSUB(256,30, -3.0) PKD(7,5,3, 0.10\,5048.0,1.00\,F,T) Exp:XDB5US
TRIANGLE LABS TextsTLI M23 BLANK TLH45399
A4.17E4
±leiU980780 #1-662 Acq:15-APX-1998 20i48i51 GC XI + Voltage SIS 70S Noime:1226
41.7428 Fi4 BSUB(256,30,-3.0) PKD(7, 5,3,0.10\,4904.0,1.00\, F,T) Exp:HDB5US
ttlANGLE LABS Text:TLI H23 BLANK TLH4S399
001 A1.01E5
411 00
O.OSO
42:00 Time
34:00 35:00 36:00 37:00 38:00 39': 00
File:V980780 #1-662 Acq: 15-APR-1998 20:48:51 SC EH- Voltage SIR 70S
430.9729 T:4 Exp:NDB5OS
TRIANGLE LABS Text-.TLI M23 BLANK TLI#45399
40:00
41:00
901
801
701
601
50.
40.
301
20.
10:
0.
41:27
.O.OEO
00 Tin
_I.7£7
,.1.SE7
.1.3X7
.1.2E7
.1. OE7
.8.3E6
.6.6E6
'•.5.0X6
.3. 3E6
.1. 7E6
rr
-r
34:00 35:00 36:00 37:00 38:00 39:00
File:U980780 #1-662 Acq:15-APX-199B 20:48:51 SC XI+ Voltage SIS 70S
513.6775 T>4 ExpsHDBSOS
TRIANGLE LABS TexttTLI M23 BLANK TLI#45399
1001
40:00
41\00
O.OEO
42 00 Time
34100
35100
36:00
37:00
38100
39:00
40100
41:00
0.0X0
42:00 Tim,
67
-------
Flla:US8O7BO tl-662 Acq: J.5-ATK-11I9B 20148151 GC EH- Voltage SIR 70S Boif»: 1211
457.7377 Ti4 BSUB(256r30, -3.0) rtO>(7,5,3, 0.10\,4844.0,1.00\rF,T) XxptmVBSOS
TRIANGLE LABS TmxtiTLI M23 BZMOC TLI945399
100\ A1.72X5
BO:
60.
40.
20.
38 12 38:18 38,24 38:30 38t36 38:42
F±l«:0980780 fl-662 Acq:15-APX-1998 20:48,51 GC XI+ Voltage SIX 70S Koim»:556
459.7348 F:4 BSOB(256,30,-3.0) PKD(7,5,3,0.10\,2224.0,1.00*,F,T) XxpiHDBSUS
XXIAIKLX LABS Text.IXJ H23 BLANK TLIf45399
A2.00X5
38t48
80.
60.
40.
20.
A9.06E3
38 12 38:18 38:24 38:30 38:36 38:42
rileiU9807BO tl-662 Acq:15-APX-1998 20:48:51 GC EI+ Voltage SIX 70S Noise:1263
469.7779 T:4 BSUB(256r30,-3.0) PKD(7,5,3,0.1Q\,5052.0,1.00\,F,T) ExptNDBSUS
TXIAHSLX LABS Toxt:TLI M23 BLANK TLI#45399
1004 A1.Q2E8
38:48
38-12 38:18 38:24 38:30 38:36 38:42
File:U9B0780 fl-662 Acq:15-APX-1998 20:48:51 GC EI+ Voltage SIR 70S Noise:SOS
471.7750 Ts4 BSUS(256,30, -3. 0) PKD(7, 5,3, 0.10\,2020.0,1.00\,F,T) Xxp:NDB5US
TRIANGLE LABS Text.-XL! H23 BLANK TLIM5399
1001 Al.,
38:48
38-12 38:18 , 38:24 38:30 38-36
FilesU980780 tl-662 Acq:15-APR-1998 20:48:51 GC XI+ Voltage SIR 70S
430.9729 F:4 XxpiSDBSVS
TRIANGLE LABS Text j 1X1 M23 BLANK TLIH5399
10 0\
ao:
60.
40.
20.
38:42
38:48
.5.3X4
'.4.3X4
.3.2X4
.2.1X4
.1.1X4
0.0X0
Time
5.1X4
4.1X4
.3.1X4
.2.1E4
.1. 0X4
0.0X0
T±*<
2.0E7
.1. 6X7
.1.2X7
.8.2X6
.4.1X6
.0.0X0
Tixe
.2.3X7
'.1.9X7
11.4X7
.9.3X6
'.4. 7X6
'.0.0X0
Tim
_1.6X7
'.1.3X7
19.7X6
.6.5X6
.3.2X6
38,12
38:18
38:24
38:30
38:36
38:42
38:48
'.0.0X0
Tim
-------
u/
CO
Peak Locate Examination:15-APR-1998:20:47 File:U980780
Experiment:NDB5US Function:2 Reference:PFK
-------
TLI Project: 45399
Client Sample: TLI M23 Blank
Method 23 TCDD/TCDF Analysis (DB-225)
Analysis File: P981305
Client Project:
Sample Matrix:
TLI ID:
Sample Size:
Dry Weight
GC Column:
r012.002/Lime Kiln
XAD
TLI Blank
1.000
n/a
DB-225
Date Received:
Date Extracted:
Date Analyzed:
Dilution Factor:
Blank File:
Analyst:
II
04/03/98
04/16/98
n/a
U980780
BJG
Spike File:
ICal:
ConCal:
% Moisture:
% Lipid:
% Solids:
SPC2NF04
PF24098
P981302
n/a
n/a
n/a
2,3,7,8-TCDF
ND
0.005
Merhai Standard
Amt
QC Limits Ratio
13C,:-2,3,7,8-TCDF
2.8
69.2
40%-130%
0.75
22:23 _
Recovery Standard
13C12-1,2,3,4-TCDD
0.78
21:17
Data Reviewer.
04/20/98
Page 1 of 1
<3NFJ>SR *ZOi LARS 6.11 JO
Triangle Laboratories, lnc.«
801 CapKola Drive • Durham, North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 21:27 04/20/9*
-------
initial
Date...
Data Review By:
Calculated Noise Area: 0.13
The Total Area for each peak with an ion abundance ratio outside
ratio limits has been recalculated according to method requirements.
Page Ho.
04/20/98
Listing of P981305B.dbf
Hatched
-------
'11»,P98130S tl-lOOt, Acq,16-APx-199B 15,42,39 11+ Voltag* Sit 7OP
03.9016 Xip:DB225
IXZAHSLX LABS TmxtiTLI M23 BIMOC TLH4S399
23t24
« 21:48 22:00 22:12 22:24 23-tf 224a
file.-PS81J05 *1-1006 Acq:16-AFR-1998 15:42:39 EI+ Voltage SIX 70P
315.9419 Exp:DB225
TRIANGLE LABS Text:TLI H23 BXJUW TLH45399
1001
9Sl
80.
75j
70:
55j
50:
55:
50.
45.
40l
3S-
30.
25.
20.
15.
10:
5.
0
22; 23
-2.5X5
.2.4X5
.2.2X5
.2.1X5
.2.0X5
.1.9X5
Ll. 7B5
.1. 6X5
.1.5X5
.1.4X5
.1.2X5
'•.JL.1X5
Ll. 0£5
.8.7X4
.7.5X4
.6.2X4
-.5.0X4
'•.3.7X4
.2.5X4
.1.2X4
21tOO 21tl2 21i24 31i36 21t48 22:00 22il2 22:24 22,36 22i48 33tOO 23tl2 23:24 23i36' 33i48'
0.0*0
Tim
-------
'ile:P9il305 tl-1006 Acq:16-APX-199B 15:43*39 SI4- Voltage SIR fOP Hoi**:41
03.9016 BSUB(256,30,-3.0) PKD(5,3,l,0.10\,164.0,0.00\,r,r) Exp:DB225
TXIANGLS LABS TmxtiTLI M23 BLANK TLH45399
003k
18'tOO 19 > 00 30': 00 21iOO 22iOO 23iOO
lle:P981305 il-1006 Aoq:16-APX-1998 15:42:39 EI+ Voltage SIX 70P Noi*m:40
05.8987 BSOB(256,30,-3.0) PKD(S,3,1,0.10*, 160.0,0.00\,r,F) Exp:DB225
TRIANGLE LABS TmxtiTLI M23 BLANK TLH45399
00*
24100
18:00 19iOO : 20:00 21tOO 22:00 23:00
•ile:P981305 U-1006 Acq:16-APR-l998 15:42:39 XI+ Voltage SIX 70P Noita:47
315.9419 BSUB(256,JO,-3.0) PXD(5,3,1,0.10\,188. 0,0.00\,r,r) Exp:DB225
TRIANGLE LABS Text!HZ H23 BLANK TLH45399
10(0. A1.10E6
80.
60.
40.
301
24:00
IB:00 19:00 20:00 21:00 22:00 23:00
r±le:P981305 il-1006 Acgtl6-APX-1998 15:42:39 EI+ Voltage SIR 70P Noif«:42
317.9389 BSUB(256,30,-3.0) PKD(5,3,1,0.10\,168.0,0.00\,F,F) Exp:DB225
TRIANGLE LABS Text:TLI H23 BLANK TLH45399
1001 A1.47E6
80.
60.
40:
20.
24 : 00
18:00 19:00 . , 20:00 21:00 22:00 23:00
rilf:P98130S il-1006 Acq:16-APS-1998 15:42:39 XI+ Voltage SIS 70P
375.8364 Exp:DB225
TRIANGLE LABS Tmxt:TLI M23 BLANK TLH45399
24:00
0.0X0
25': 00 Tim*
.O.OEO
25:00 Time
.2.5X5
-2.0E5
L1.5ES
.9.9E4
'.5. OE4
O.OEO
25tOO Ti*
-3.3ES
-2.6ES
-2.0ES
.1.3E5
.6.6E4
O.OEO
25:00 Tim
20:3020:5521:20 33.70
31:4523'10
18:00
19:00
20:00
21:00
22iOO
23:00
24:00
25:00
-------
19:00 20:00 21:00 22:00
il»:P98130S #1-1005 Adj: 16-APR-199 8 15:42:39 EI+ Voltage SIR 70P Hoi»»:34
21.8936 BSUB(256,30,-3.0) PKD(S,3,1, 0.10\,136.0,0,00\,r,f) Xxp:DB22S
TRIANGLE LABS Text.IIJ M23 BLANK TLIM5399
.J.»sP98130S tl-1000 Acq:16-APR-1998 15:41:J» IX* Voltage SIM 70F
19.8965 BSVB(256,30r-3.0) PKD(5,3,1,0.10\,160.0,0.00\,T,T) Xxp:DB225
IAOGLX LABS TuxtiXLI H23 BLANK TLH45399
004
t 0.0*0
24i00 T±m»
80.
60.
40.
20.
A865.02
19,00 20:00 21*00 22:00 23:00
rile:P981305 #1-1005 Acq:16-APS-1998 15:42:39 EH- Voltage SIR 70P Woiae:47
27.8847 BSUB(256,30,-3.0) PKD(S, 3,1, 0.10\, 188.0,0. 00\,rrF) EzpsDB22S
TRIANGLE LABS ToitlTLI M23 BLAST TLH4S399
1001 A1.75E6
so:
60.
40.
20.
O.OEO
24:00 Tim
19t00 20:00 21:00 22:00 23:00
rile:P98130S #1-1005 Acqil6-APR-1998 15:42:39 EI+ Voltage SIR 70P Noiae,54
331.9368 BSUB(2S6,30,-3.0) PKD(5,3,l,0.10\r216.0,0.00\,T,T) Exp:DB22S
TRIANGLE LABS Text:HI M23 BLANK TLH45399
100S A1.21E6
80.
60.
40.
20.
A7.96E5
19:00 20:00 21:00 22:00 23:00
rilo>P981305 #1-1005 Acqrl6-APR-1998 15:42:39 XI* Voltage SIS 70P Noiaa:43
333.9338 BSUB(256,30, -3. 0) PKD(5, 3,1, 0.10\,172.0, 0.00\,F,F) ExpiDB225
TRIANGLE LABS TexttZLX M23 BLANK TLI045399
1004 A1.55X6
BO:
60.
40.
20.
0.
Al.02E6
24 : 00
241 00
'.3. SE5
'.2.6E5
.1. 7E5
'.8.7E4
O.OEO
Tim
.2.ass
-2.3E5
-1. 8ES
-1.2E5
-5 . 9X4
.0. OEO
Tim
.3.7ES
.3. OE5
.2.2X5
.1.5X5
.7.4X4
0.0X0
19100
20,iOO
21100
22: OH
23:00
24:00
-------
Tlle,P981305 tl-1006 Acq:16-APX-1998 lit42,39 11+ Voltage SIR 70P
303.9016 Exp:DB225
TRIANGLE LASS Text:TLI H23 BLANK TLH45399
100J
80:
60.
40.
20.
17>54
i'f 32 19't3620:01
2 As 3
20,59
21159
21:38
22134
22t49
23114
23,53 24,28
rr
T
18:00 19:00 20:00 21:00 22:00 23:00
Flle,P98130S tl-1006 Acq:16-APR-1998 15,42,39 EI+ Voltage SIX 70P
315.9419 Exp:DB225
TRIANGLE LABS Teit:TLI M23 BLANK TLH45399
1003
80:
50:
40:
20.
24,00
25,00 Time
.2.5X5
.2.0X5
'.1.5E5
ll.OSS
T
T
rr
T
T
O.OEO
18:00 19:00 20:00 21:00 22:00 23:00 24:00
File:P981305 tl-1006 Acq:16-APX-1998 15:42:39 Eli- Voltage SIX 70P
319.8965 Exp,DB225
TRIANGLE LABS Text .-HI H23 BLANK TLIt45399
1003
80:
50:
40:
20:
0.
18:00 19:00 20:00 21:00 22:00 23:00
rile:P981305 tl-1006 Acq:16-APR-1998 15:42:39 EI+ Voltage SIX 70S
331.9368 Exp:DB225
TRIANGLE LABS Teit-.TLI H23 BLANK TLIt45399
17:59
18:57
19:38
20:20
20:45
21:49
22:24
23:21
24,01
24,25
-r
-r
~r
~r
T"
2*1-00
25:00 Time
-8.8E2
7.1E2
.5.3E2
-3.SE2
.1.8E2
O.OEO
25:00 Tine
loot
so:
50:
40:
20:
18:00 19:00 20:00 21:00 22:00 23:00 24:00 25:00 Time
rlle:P981305 tl-1006 Acg:16-APR-1998 15:42:39 K+ Voltage SIR 70P
292.9825 Eip:DB225
TRIANGLE LABS TextiZLT H23 BLANK XLHH5399
18:26 19:21 19:59 21:09^21:35 22:12 22±4_
21:17
21:00
.2.9E5
-.2.3E5
Ll. 8E5
.1.2E5
.5.9E4
•.O.OEO
18:00 19:00 20:00 21:00 22': 00
rile:P981305 tl-1006 Acq:16-APX-1998 15:42,39 EI+ Voltage SIX 70P
330.9792 Exp:DB225
TRIANGLE LABS Text:TLI K23 BLANK TLIt45399
23:00
24,00
O.OEO
25:00 Time
1l0oL^y^^^>>^r^
60:
40:
20:
.5.1X5
.4.1X5
.3.1X5
la. 0x5
ll.OES
18:00
19,00
20:00
21,00
22,00
23:00
24:00
.0.0X0
25,00 Tim*
-------
Ref, uss 292,9825 Peak top
Height ,87 volts Span 288 ppi
Systei file naie
Oka file rate
Resolution
Group nmber
lonlzatlon lode
Switching
Ref, lasses 292,9825,
A--P981385
fl 292,9825
B 383,9816
COAC 000^
vwiOw/
0 315,9419
E 317,9389
F 319,8965
8 321,8936
H 327,8847
I 338.9792
J
K
L
H
1
El*
VOLTRGE
388,9781
338,9792
331,9368
333,9338
375,8364
ChameL I 338.9792 Peak top
Height ,87 volts Span 288 ppi
-------
Pages 77 through 130 from the Triangle Laboratories, Inc. analytical report
have been excluded by PES since these pages present results for samples
collected at another lime kiln facility during the same mobilization.
-------
TLI Project: 45399
Client Sample: M23-I-3
Method 23 PCDD/PCDF Analysis (a)
Analysis File: T981957
Client Project:
Sample Matrix:
TLI ID:
Sample Size:
Dry Weight:
GC Column:
r012.002/Lime Kiln
M23
204-92-3A-D
1.000
n/a
DB-5
Date Received:
Date Extracted:
Date Analyzed:
Dilution Factor:
Blank File:
Analyst:
04/01/98
04/03/98
04/18/98
n/a
U980780
HLM
Spike File:
ICal:
ConCal:
% Moisture:
% Lipid:
% Solids:
SPMIT204
TF51308
T981946
n/a
n/a
n/a
Anatytes
2,3,7,8-TCDD
1,2,3,7,8-PeCDD
1,2,3,4,7,8-HxCDD
1,2,3,6,7,8-HxCDD
1,2,3,7,8,9-HxCDD
1,2,3,4,6,7,8-HpCDD
1,2,3,4,6,7,8,9-OCDD
2,3,7,8-TCDF
1,2,3,7,8-PeCDF
2,3,4,7,8-PeCDF
1,2,3,4,7,8-HxCDF
1,2,3,6,7,8-HxCDF
2,3,4,6,7,8-HxCDF
1,2,3,7,8,9-HxCDF
1,2,3,4,6,7,8-HpCDF
1,2,3,4,7,8,9-HpCDF
1,2,3,4,6,7,8,9-OCDF
Totals''' -:':.::%'';: ::••::.:.::;'>;
Total TCDD
Total PeCDD
Total HxCDD
Total HpCDD
Total TCDF
Total PeCDF
Total HxCDF
Total HpCDF
Anrt, (ng)
ND
ND
ND
ND
ND
ND
EMPC
0.02
ND
ND
EMPC
EMPC
ND
ND
0.009
ND
ND
: 'v^/vAmtMngJ
0.01
ND
ND
ND
0.11
0.02
0.01
0.009
--' tit £l»PO '
0.003
0.004
0.007
0.007
0.007
0.01
0.03
0.003
0.003
0.007
0.004
0004
\/.V/\^T
000*5
v.v/\y«/
0008
u.v/v/o
002
\J.\J ^
Number DL EMPC
2
0.004
0.007
0.01
10 0.12
1
1 0.02
1
fcalfo « ftt..-- Flag*
——^
JB_
0.82 25:26 B_
FI
J_
i (v; •3^-/iQ T
i.uo jj.oy j
flags
n
Page 1 of 2
Mm_PSR vl.04, LARS 6.11.00
Triangle Laboratories, Inc.®
801 Capitola Drive • Durham, North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 15:38 04/20/98
\o •*•
-------
TLI Project: 45399
Client Sample: M23-I-3
Method 23 PCDD/PCDF Analysis (a)
Analysis File: T981957
Internal Standards - -
13C12-2,3,7,8-TCDF
13C12-2,3,7,8-TCDD
13C,2-l,2,3,7,8-PeCDF
13C,2-l,2,3,7,8-PeCDD
13C,2-l,2,3,6,7,8-HxCDF
13C12-l,2,3,6,7,8-HxCDD
13Ci2-l,2,3,4,6,7,8-HpCDF
13C12-l,2,3,4,6,7,8-HpCDD
13C,2-1,2,3,4,6,7,8,9-OCDD
Surrogate Standards (Type A)
13C,2-2,3,4,7,8-PeCDF
13C,2-l,2>3,4,7,8-HxCDF
13C,2-l,2,3,4,7,8-HxCDD
13C,2-l,2,3,4,7,8,9-HpCDF
Other Standard^ :;
37CL,-2,3,7,8-TCDD
Alternate Standards (Typk A}: ,:;.;
13C,2-l,2,3,7,8,9-HxCDF
nCu-23,4,6,l,8-H\CDlr
Recovery Standards
13C,2-1,2,3,4-TCDD
13C,2-l,2,3,7,8,9-HxCDD
Ami (ngj >
3.1
2.9
2.9 "
3.2
4.1
3.7
40
40
5.3
Atwu (&g)
3.8
3.5
3 6
2.7
Amt, (ritj) •
3.4
Amt. {n{j):;':.. ?•
3.2
3.8
f;^ R«*V»ry
76.6
71.7
72.6
80.1
101
93.2
99 8
101
65.6
% Recovery
94.9
87.6
90 R
68.1
% Recovery
84.9
•'. _;;^. Recovery1':
80.1
94.0
s SR vUX. LARS 6.11OO
Printed: 15:38 04/20/98
132
-------
Initial
..Date..
Data Review By:
¥ Calculated Noise Area: 0.16
The Total Area for each peak with an ion abundance ratio outside
ratio limits has been recalculated according to method requirements.
Page No.
04/20/98
Listing of T981957B.dbf
Hatched GC Peaks / Ratio / Ret. Time
Compound/
M_Z QC.Log Omit Why . .RT. OK Ratio Total.Area... Area.Peak.1.. Area.Peak. 2. . Rel.RT Conpound. Name. . ID.. Flags.
TCDF
304-306
A
M
A
304-306
13C12-TCDF
316-318
316-318
TCDD
320-322
D
D
0.65-0.89
DC NL 0:
22:
22:
23:
23:
23:
24:
24:
24:
25:
25:
25:
25:
26:
00
12
42
00
21
39
04
22
48
01
13
26
52
04
0.
0.
RO 0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
RO 0.
RO 0.
70
74
63
82
83
86
68
89
72
79
85
82
63
56
13 Peaks
0.46
0.80
0.60
0.69
3.06
2.19
2.03
1.66
2.63
1.92
0.85
3.96
1.20
0.94
22.53
0
0
0
1
1
0
0
1
0
0
1
0
0
.34
.26
.31
.39
.01
.82
.78
.10
.85
.39
.79
.52
.41
0.65-0.89
DC NL 0:
DC WL 24:
24:
24:
25:
25:
00
22
38
59
24
51
RO 1.
0.
0.
0.
0.
RO 0.
4 Peaks
11
81
88
36
75
58
0.34
1.52
0.75
2.59
595.24
2.25
600.83
tttr*T\v I
0.65-0.89
DC NL 0:
23:
23:
DC SN 24:
DC SN 24:
DC SN 24:
DC SN 24:
DC SN 24:
D SN 24:
D SN 25:
DC SN 26:
00
34
58
04
13
17
20
31
58
24
03
0.
0.
0.
RO 1.
0.
RO 0.
0.
RO 0.
RO 0.
RO 1.
RO 1.
83
82
79
00
83
25
75
60
59
19
93
0.22
1.04
0.68
0.12
0.11
0.07
0.14
0.07
0.51
0.48
0.27
0
1
254
0
.35
.20
.91
.98
0.
0.46
0.41
0.38
1.67
1.18
1.21
0.88
1.53
1.07
0.46
2.17
0.82
0.73
0.
0.40
1.39
340.33
1.68
868-1.077
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
1.
1.
1.
961-
0.
0.
0.
0.
1.
1.
000
874
894
906
919
931
948
959
976
985
993
001 2378-TCDF AN
018
026
1.039
000
959
970
984
000 13C12-2378-TCDF ISO
018
J
J
J
J
J
J
J
J
J
J
J
J
0
0
.47
.30
0.
0.57
0.38
896-1.045
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
000
902
917
921
927
929
931
938
955
972
997
J
J
320-322
37C1-TCDD
328
2 Peaks
DC NL
0:00
1.72
0.13
0.924-1.076
0.000
Triangle Laboratories, Inc.® Analytical Services Division
801 Caprtola Drive • Durham, North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 15:39 04/20/98
-------
Page No.
04/20/98
Listing of T981957B.dbf
Hatched GC Peaks / Ratio / Ret. Time
Compound/
M_Z.... QC.Log omit Why ..RT. OK Ratio Total.Area... Area.Peak.1.. Area. Peak.2.. Rel.RT Compound.Name.. ID.. Flags.
328
13C12-TCDD
332-334
332-334
PeCDF
340-342
D
D
D
D
D
D
340-342
13C12-PeCDF
352-354
352-354
PeCDD
356-358
356-358
DC
DC
D
D
DC
DC
D
D
D
D
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
3
NL
4
NL
SN
SN
SN
SN
SN
SN
SN
SN
SN
SN
SN
1
NL
6
NL
SN
SN
SN
SN
SN
WH
0
24:45
26:09
26:33
Peaks
0:00
24:57
25:57
26:08
26:29
Peaks
0:00
27:24
28:24
28:33
28:43
29:03
29:08
29:25
30:07
30:16
30:31
30:42
31:10
Peak
0:00
28:31
29:24
29:41
30:06
30:27
31:04
Peaks
0:00
28:54
29:24
29:57
30:28
30:36
31:15
Peaks
0.
RO
RO
1.
RO
RO
RO
RO
RO
RO
RO
1.
RO
RO
RO
RO
1.
RO
RO
RO
RO
RO
RO
RO
4,
380
1
385
.06 4.06
.48 380.48
.37 1.37
.91
65-0.89
2.
0.
0.
0.
0.
32-
0.
1.
1.
1.
1.
1.
0.
2.
1.
1.
0.
0.
0.
44
69
79
79
63
1.78
73
73
48
46
37
28
86
08
55
50
24
60
30
0
1
524
430
5
962
itipm
llvLfl
0
0
0
2
0
0
0
0
0
0
0
0
0
2
.64
.96 0.80
.48 232.14
.90 190.13
.06 2.20
.40
/T>Q/** Tiff IPnl 1 1-rtJC
.18
.82
.52
.19 1.30
.45
.38
.41
.64
.79
.70
.07
.10
.20
.19
32-1.78
0.
1.
1.
1.
1.
0.
1.
82
39
46
22
47
89
07
0
3
470
4
448
1
1
928
D&/~TV
.32-1.78
1.
22
0.45
2.
24
0.82
1.05
2.17
1.10
0
0
0
0
0
0
0
0
.15
.25 1.89
.54 279.61
.05 2.46
.35 266.76
.58 0.96
.07 0.65
.84
.18
.15
.43
.23
.33
.15
.18
.00
0
1
1
.947
.001 37C1-TCDD
.016
CLS
0.924-1.076
0
1.16 0
292.34 0
240.77 1
3.48 1
.000
.955
.993 13C12-1234-TCDD
.000 13C12-2378-TCDD
.013
RSI
IS1
0.926-1.063
0
0
0
0.89 0
0
0
0
1
1
1
1
1
1
0.864
0
1.36 0
190.93 1
2.02 1
181.59 1
1.08 1
0.61 1
.000
.932
.966
.971
.977
.988
.991
.001 12378-PeCDF
.024 23478-PeCDF
.029
.038
.044
.060
-1.136
.000
.970
.000 13C12-PeCDF 123
.010
.024 13C12-P6CDF 234
.036
.057
AN
AN
IS2
SUR1
0.936-1.021
0
0
0
0
1
1
1
.000
.949
.966
.984
.001 12 3 7 8- PeCDD
.005
.026
AN
Triangle Laboratories, Inc.® Analytical Services Division
801 Capitola Drive • Durham, North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 15:39 04/20/98
1 ?
-------
Page No.
04/20/98
Listing of T981957B.dbf
Hatched GC Peaks / Ratio / Ret. Time
Compound/
M_Z.... QC.Log omit Why ..RT. OK Ratio Total.Area... Area.Peak.1.. Area.Peak.2.. Rel.RT Compound.Name.. ID.. Flags.
13C12-PeCDD
368-370
368-370
HxCDF
374-376
374-376
13C12-HXCDF
384-386
DC
NL
2
1.32-1.78
0:00 RO 1.00
30:27 1.50
30:35 1.51
Peaks
Aln»»rA .
1.05-1.43
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
NL
SN
SN
SN
SN
SN
SN
SN
SN
SN
SN
3
NL
0:
31:
32:
32:
32:
33:
33:
33:
33:
34:
34:
34:
34:
34:
00
55
04
52
59
04
09
27
59
05
10
11
19
22
RO
RO
RO
RO
RO
RO
RO
RO
RO
1.
1.
1.
1.
0.
2.
2.
0.
1.
8.
1.
a.
i.
0.
17
07
13
00
83
40
17
48
31
50
58
50
13
24
Peaks
0:
31:
00
54
0.
RO
32:02
32:52
32:58
33:16
DC
SN
33:
:27
33:51
0.16
287.92 172.70
30.16 18.15
318.08
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
2.
39
31
96 0.51
67 0.37
45 0.25
11
13
25
30
09
27
09
32
22
08
43-0.59
1.
0.
0.
0.
0.
00
58
54
51
51
0.49
0.51
RO
33:56
384-386
HxCDD
390-392
DC
DC
DC
DC
DC
DC
DC
DC
11
NL
SN
SN
SN
SN
SN
SN
SN
34
34
34
34
:03
:12
:30
:34
RO
RO
RO
2.33
0.47
0.
0
1
.82
.51
.23
0.69
Peaks
0
32
33
33
33
33
33
33
:00
:53
:04
:17
:21
:27
:40
:57
1
RO
RO
RO
RO
RO
RO
.05-1.43
1
1
0
0
1
1
1
0
.25
.95
.94
.57
.20
.89
.50
.77
0.18
2.
61 0.96
2.17 0,76
308.
366.
.75 103.87
.31 123.43
1.71 0.56
320.32 108.66
0
1
0
211
1
2
1,218
.09
.19 0.38
.51 0.28
.70 71.14
.12 0.91
.40 1.09
.79
0.869-1.131
0.000
115.22 1.000 13C12-P«CDD 123 IS3
12.01 1.004
0.963-1.045
0.
0.
0.45 0.
0.37 0.
0.30 1.
1.
1.
1.
1.
1.
1.
1.
1.
1.
000
968
973 J
997 123478-HXCDF AN J
001 123678-HxCDF AN J
003
006
015 234678-HxCDF AN
031
034
036
037 123789-HxCDF AN
041
042
0.879-1.121
0
1.65 0.
1.41 0
204.88 0
242.88 1
1.15 1
211.66 1
1
0.81 1
0.34 1
140.56 1
0.74 1
1.59 1
.000
.968
.972
.997 13C12-HXCDF 478 SUR2
.000 13C12-HXCDF 678 IS4
.009
.015 13C12-HXCDF 234 ALT2
.027
.029
.033
.037 13C12-HXCDF 789 ALT1
.047
.049
0
0
0
0
0
0
0
0
.45
.45
.29
.14
.33
.40
.27
.36
0.958
0
0
0
0
0
0
1
1
-1.013
.000
.977
.983
.989
.991
.994
.000 123678-HxCDD AN
.009 123789-HxCDD AN
Triangle Laboratories, Inc.® Analytical Services Division
801 Capitola Drive • Durham, North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 15:39 04/20/98
-------
Page No.
04/20/98
Listing of T981957B.dbf
Matched GC Peaks / Ratio / Ret. Time
Compound/
M_Z QC.Log Omit Why ..RT. OK Ratio Total.Area... Area.Peak.1.. Area.Peak.2.. Rel.RT Compound.Name.. ID.. Flags.
D
390-392
13C12-HXCDD
402-404
402-404
DC
DC
DC
DC
D
DC
DC
DC
DC
DC
DC
DC
DC
SN
SN
SN
SN
SN
WH
WH
WH
WH
0
NL
SN
SN
SN
5
33:
34:
34:
34:
34:
34:
34:
34:
34:
59
00
03
04
06
13
17
18
27
RO
RO
RO
RO
RO
RO
RO
RO
RO
0.
5.
0.
0.
0.
1.
0.
0.
2.
50
33
88
67
59
98
49
72
36
Peaks
0:
33:
33:
33:
33:
33:
33:
33:
34:
00
04
14
21
27
34
39
57
14
1.
RO
RO
RO
RO
RO
0.
0,
0,
0
0
0
0
.22
.07
.13
.18
.42
.99
.40
0.33
0
0
.74
.00
05-1.43
0.
1.
0.
0.
0.
1.
1.
1.
7.
66
39
32
20
45
20
21
21
37
Peaks
0
1
0
0
0
196
258
275
0
732
ro • Hvmi
.42
.41
.13
.20
.25
.41
.67
.33
.85
.67
n / Hnr
1.
1.
1.
1.
1.
1.
1.
1.
1.
010
010
012
012
013
017
019
019
024
0.970-1.030
0.
0.82 0.59 0.
0.
0.
0.
107.29 89.12 0.
141.87 116.80 1.
150.63 124.70 1.
2.80 0.38 1.
000
983
988
991
994
998 1
000 1
009 1
017
998 13C12-HXCDD 478 SUR3
000 13C12-HXCDD 678 IS5
009 13C12-HXCDD 789 RS2
HpCDF
408-410
408-410
13C 12 -HpCDF
418-420
418-420
HpCDD
424-426
424-426
13C12-HpCDD
436-438
436-438
DC NL 0:00
35:49
DC SN 36:14
1 Peak
DC NL 0:00
35:49
37:19
DC SN 37:37
DC SN 37:47
2 Peaks
DC NL 0:00
DC SN 36:50
0 Peaks
DC NL 0:00
36:50
DC SN 37:19
1 Peak
0.88-1.20
RO 1.70
1.06
1.00
0.37-0.51
RO 1.27
0.43
0.42
RO 0.19
0.45
0.88-1.20
0.91
RO 1.80
0.88-1.20
1.00
1.02
RO 0.78
0.20
0.64 0.33
0.34
0.64
0.22
203.28 61.31
100.06 29.43
0.49
0.29
303.34
0.21
0.31
0.00
0.30
168.34 84.95
0.35
168.34
0.996-1.047
0.000
0.31 1.000 1234678-HpCDF
1.012
0.944-1.112
0.000
141.97 1.000 13C12-HpCDF 678
70.63 1.042 13C12-HpCDF 789
1.050
1.055
0.976-1.005
0.000
1.000 1234678-HpCDD
0.973-1.027
0.000
83.39 1.000 13C12-HpCDD 678
1.013
AN
IS6
SUR4
AN
IS7
Triangle Laboratories, Inc.® Analytical Services Division
801 Cap'rtola Drive • Durham, North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 15:39 04/20/98
1 o
-------
Page No.
04/20/98
Listing of T981957B.dbf
Hatched GC Peaks / Ratio / Ret. Time
Compound/
M_Z.... QC.Log Omit Why ..RT. OK Ratio Total. Area... Area.Peak.1.. Area.Peak. 2.. Rel.RT Compound.Name.. ID.. Flags.
OCDF
442-444
442-444
OCDD
458-460
M
458-460
13C12-OCDD
470-472
470-472
DC
DC
DC
DC
DC
NL 0:00
SN 40:35
SN 41:37
0 Peaks
NL 0:00
40:23
i Peak
NL 0:00
40:23
1 Peak
0.76-1.02
0.85
0.82
0.78
0.76-1.02
0.83
RO 1.06
0.76-1.02
RO 1.45
0.86
Above: HpCDD / Octa-CDD and CDF Follows
0.24
0.40
0.16
0.00
0.22
0.59
0.59
0.21
147.85
147.85
0.33
68.35
0.901-1.099
0.000
1.005 OCDF
1.031
0.901-1.099
0.000
0.31 1.000 OCDD
0.996-1.004
0.000
79.50 1.000 13C12-OCDD
AN
IS8
Column Description.
"Why" Code Description QC Log Desc.
M_Z -Nominal Ion Mass(es)
..RT. -Retention Time (mm:ss)
Rat.l -Ratio of M/M+2 Ions
OK -RO=Ratio Outside Limits
Rel.RT-Relative Retention Time
End of Report ***
WL-Below Retention Time Window
WH-Above Retention Time Window
SN-Below Signal to Noise Level
-------
File:T981957 #1-720 Acq:18-APR-1998 06:12:52 EI+ Voltage SIR
303.9016 F:2 BSUB(256,30r -3.0) PKD(9, 5,5,0. 05\r380. 0,1. 00\,F,
70T Noiae:95
T) ExpsKOBSUS
TRIANGLE LABS Text:M23-I-3 TLIV45399 HKT. TIME » 06:13
1001
80:
60:
40:
20:
0'
Al . 39E4
n
Al.
A8.53E3
A7.84E3 A
Jl A1.01E4 . A ' (1
/LwkH^/V^
23*00
.A/IMJUI
24:00 25:00
F±le:T981957 #1-720 Acq:18-APR-1998 06:12:52 SI+ Voltage SIR
'9E4 3.5E3
A5.21E3
\.^J W V-J«^v^-^AwvswV'Lv>~»-^
-2.8E3
-2.1E3
_1 . 4E3
.7.1S2
• n nvn
'26:00 271-00' ' ' ' Time
70T Noise -.136
305.8987 F:2 BSUB( 256, 30, -3. 0) PKD(9, 5,5, 0 .05\,544 .0 , 1.00\,F,T) ExpsNDBSUS
TRIANGLE LABS Text:M23-I-3 TLIt45399 INJ. TIME - 06:13
1001
80:
60:
40:
20:
0'
A1.67E4
*
f\
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315.9419 F:2 BSUB(256, 30, -3 . 0) PKD( 9, 5,5, 0. 05%, 412. 0, 1 . 00\,F ,
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'261-00 27l-0o' ' ' Time
70T Noise: 10 3
T) ExpiNDBSVS
TRIANGLE LABS Text:M23-I-3 TLH45399 INJ. TIME - 06:13
1003
80:
60:
40:
20:
0.
-
231-00
*2.5
/
24 .- 00 25 ': 00
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JE6 6.8E5
'-.5.5E5
^4.1E5
.2.7E5
-1.4E5
O.OEO
26.' 00 271-00 ' Time
70T Noise: 96
317.9389 F:2 BSUBf 256,30, -3:0) PKD<9, 5,5, 0. 05%, 384. 0,1. 00%,f, T) ElpiNDBSUS
TRIANGLE LABS Text.-Af23-.T-3 TLI#45399 INJ. TIME = 06:13
1003
aol
601
40:
20:
ol
23\00
A3.4
1
24\00 25 1-00
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TRIANGLE LABS Text:M23-I-3 TLIH45399 INJ. TIME « 06:13
1003
80.
60.
40.
20.
0.
^^^ _2^J^_23jj04_^23jJ2^
23:00
23:54 24:28 25:02
24:00 25:00
File:T981957 #1-720 Acq:18-APR-1998 06:12:53 EI+ Voltage SIR
375.8364 F:2 Exp:NDB5US
25:39 25j59 26:25 26:45 27:07 ^1.6E6
'V" N/
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.9 . 7E5
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70T
TRIANGLE LABS Teit:M23-I-3 TLI#45399 INJ. TIME - 06:13
100J
SO.
60:
401
201
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- - 23
22:42 23:08
i2:JJi Jl 1 i' Jl 11
23 .' 00
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24:17
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1 24:49 ^:23 , 26:25
1 1 24:051 24:39\ 1 , .A
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24:00 25:00
25:4I26.07 1 I 26-49 27:13 i
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138
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File:T981957 #1-720 Acq:18-APR-1998 06:12,52 EI+ Voltage SIR 70T NoiaeiSO -» 1 j /» \ lV »
319.8965 F:2 BSOB(256,30, -3.0 ) PKD(7,5, 3, 0.05\,200 .0,1.00\,T,T) Exp-.NDBSUS * \C i 7>T '+*' ' *
TRIANGLE LABS Text:M23-I-3 TLI#45399 INJ. TIME' 06:13°''
1004
flOJ
60J
40.
2(1
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26:00
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• 2 9E2
- n /lEisi
27:00 Time
File:T981957 #1-720 Acq:18-APR-1998 06:12:52 EI+ Voltage SIS 70T Noise: 59
321.8936 F:2 BSOS(256,30, -3.0) PKD(7, 5, 3,0 .051,233.0, 1.00*,F,T) Exp:NDBSUS
TRIANGLE LABS Text:M23-I-3 TLI#45399
1003
801
601
401
201
o:
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4.
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A3 . 83E3
M ' A3. 69E3
-SW wJ^AA^\/tf^
241-00 251-00
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A4.
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26:00
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1 A2.64E3
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.9.0E2
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ft nvn
— i — i — i — i — i — i — i i — i — i i "• >»•«"'
27:00 Time
File:T981957 #1-720 Acq:18-APR-1998 06:12:52 EI+ Voltage SIR 70T Noise: 4 38
331.9368 F-.2 BSUB(256, 30, -3. 0) PKD(7, 5,3,0 .051,1752
0,1.004,F
TRIANGLE LABS Text:M23-I-3 TLI#45399
1003
80.
60.
40.
20.
0
24-00 251-00
A2
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T) Exp-.NDBSUS
INJ. TIME = 06:13
<2E6 r6.4E5
Al.
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26:00
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27:00 Time
File:T981957 #1-720 Acq:18-APR-1998 06:12:52 EH- Voltage SIR 70T Noiae:182
333.9338 F:2 BSUB(256, 30, -3 .0) PKD(7, 5,3, 0. 05%, 728. 0,1 . 00\,F,T) Exp-.NDBSUS
TRIANGLE LABS Text:M23-I-3 TLI#45399
1003
a 01
601
401
201
0
24 .-00 , 251-00
A2.
1
INJ. TIME = 06:13
>2E6 r8.1E5
A2.
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26-00
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A
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27:00 Time
File:T981957 #1-720 Acq:18-APR-199B 06:12:52 EI+ Voltage SIR 70T Noise:63
327.8847 F:2 BSUB(256, 30, -3 . 0 ) PKD( 7, 5, 3, 0. 05%, 252. 0, 1 . 00%,F, T) Exp-.NDBSUS
TRIANGLE LABS Text:M23-T-3- TLI#45399
1003
801
601
401
201.
o:
24:00 25:00
INJ. TIME - 06:13
A3
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}OE6 9.8E5
ft
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•-2.0E5
• n nrn
26:00 27:00 Time
File:T981957 #1-720 Acqil8-APR-1998 06:12:52 EI+ Voltage SIR
330.9792 F:2 Exp-.NDBSUS
TRIANGLE LABS Text:M23-I-3 TLI#45399
1001
flOJ
60J
40J
20:
0
70T
JWJ. TIME - 06:13
I 33L54 24:2824:43 25^0225:17 25^39 25^59
' '
24:00 25:00
X"
26:25 26: f 5 27fQ7_ 1.6E6
^ ^,
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.9 . 6E5
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26:00 ' 27:00 ' ' ' Time
-------
File:T981957 #1-720 Acq:18-APR-1998 06:12:52
EI+ Voltage SIR 70T Koiae:54
339.8597 F:2 BSUB(256,30,-3 .0) PKD(7,5,3,0.05\,216.
TRIANGLE LABS Text:M23-I-3 TLI045399
1003
sol
60:
40:
20.
0:
A1.3
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0,1.00\,F,T) Elp-.ODBSUS
INJ. TIME - 06:13
1 I \ A5.23E3 A4.
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28:00 '
A2.5BE3 A2.
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File:T981957 tl-720 Acq:18-APR-1998 06:12:52
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V ^y^vhAvWVWN^^A-^^
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O.OEO
30\00 3l':00 ' ' ' Time
EH- Voltage SIR 70T Hoiae:77
341.8567 F:2 BSUB(256,30, -3.0) PKD(7,5,3r 0. 05%, 308.
TRIANGLE LABS Text:M23-I-3 TLI#45399
1003
sol
60:
40l
2Q-
A8.
•
A A1.28E3
1 \ inr rn ft M H
'^l-J/V^/rt^^/W/VuV T
28:00 '
18E3
0,1.00\,F,T) Exp:NDB5US
I1KT. TIME - 06:13
1 . 9E3
A2.55E3
1
A2.
Al . 60E3 i
90E3
A . Ir
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29': 00
File:T981957 #1-720 Acq:18-APR-1998 06:12:52
_1 . 5E3
_1 . 1E3
-7.SE2
1 7fO
301-00 31:00 ' ' ' Time
EI+ Voltage SIR 70T Noise: 44
351.9000 F:2 BSUB(256, 30, -3 . 0) PKD(7, 5, 3, 0 .051,176 .
TRIANGLE LABS Teit:M23-I-3 TLI#45399
1003
sol
60:
40:
20:
oj
28: 00
A2.
1
29 • 00
File:T981957 #1-720 Acq:lB-APR-1998 06:12:52
o,i.oo*,F,T) Eip-.masus
INJ: TIME - 06:13
10E6 A2.t
v ^
>7E6 8.3E5
\^
-6.6E5
-5.0E5
-3.3E5
_1 . 7E5
O.OEO
30 1- 00 31 1-00 ' ' Time
EI+ Voltage SIR 70T Noise: 55
353.8970 F:2 BSUB(256,30, -3 .0) PKD(7 ,5,3,0 .051,220 .
TRIANGLE LABS Text:M23-I-3 TLI#45399
1003
B0\
60:
40:
20:
ol
28:00
Al.
251-00
File:T981957 #1-720 Acq: 1B-APR-1998 06:12:52
330.9792 F:2 Exp:NDB5OS
0,1.00%,f,T; Exp:NBB5US
INJ. TIME =06:13
!E6 Al
1
32E6 5.7E5
I
-4.6E5
.3.4E5
-2.3E5
-1.1E5
a . nrn
30:00 31:00 Time
EI+ Voltage SIR 70T
TRIANGLE LABS Text:M23-I-3 TLI#45399
1003
80.
60.
40.
20.
0.
27:4.0 . 28:04 28:27 28^5 2S :
28:00
INJ. TIME = 06:13
04 29:20 29:47
25:00
F±le:T981957 #1-720 Acq:18-APR-1998 06:12:52
409.7974 F:2 Ezp-.NDBSUS
30:18 30:43 tl-14 ^1 . 6E6
'•i— - ^-i-»— .._,^nni ,i_^iii_n i "
.1 . 3E6
-9.7ES
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-3.2E5
O.flro
30:00 31:00 Time
EI+ Voltage SIR 70T
TRIANGLE LABS Tait:M23-I-3 TLI#45399
1003
80:
60.
40:
20:
ol
28:19
27:50 \
i .11 A Ai - fl in , t iliAl /
W^VVvvV^V^ IT
28-00
lfl 29:
" V/'u''*' T» \
\3
U.JV
fVT 1
25:00
INJ. TIME - 06:13
29:32
^ULvW
» r wy i
ri.2r3
30:15
1 31:11
if • 30:50 A I
Vv^^Aj^ilV
1 • vv » *v ^ wv-^V ^
.9.4E2
-7.0E2
-4.7E2
-2.3E2
a.OF.n
30. -00 31:00 Time
140
-------
Fi±e:tSB19S7 #1-720 Acq:l8-APR-l99B 06:13:52 Xl-t- Voltage SIS /Of Jfei»e.-56 ; 1
355.8546
Fs2 BSUB(256,30,-3.0) PKD( 7,5,3, 0. 05%, 224. 0,1. 00%, F,T) Ejcp:NDB5US
TRIANGLE LABS Text.-M23-.T-3 TLI#45399 INJ-. TIME - 06:13
1001
80.
60.
40.
20.
0.
J
*J
A3.78E3
i
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1
A1.66E3 \\A1.67E3 A1.44E3 *a.«2M
»858.89 | / 1 /\A k K M KHSJ6.33 (I A? J. R All U
v w vv vn vAr *^\/ V n i V V r ^\ W lr U M V \ JV/
pl . 4JT3
.1.1£3
.8.3E2
15.5£2
.2.BE2
28:36 281-48 2$ToO 29\12 29\24 29:36 29:48 30:00 30-12 30:24 30l-J6 30:48' 3li 00 ' 3lVl2' 31:24 rime
File:T981957 #1-720 Acq:18-APR-199B 06:12:52 EI+ Voltage SIR 701 Noise: 47
357.8516 1:2 BSUB(256,30, -3 .0) PKD(7,5,3, 0. 05\,188. 0,1. 00\,F, T) ExpsKDBSUS
TRIANGLE LABS Teit:M23-I-3 TLI#45399 TJCJ. TIME - 06:13
1001
80.
60.
40.
20.
0.
A7.
i
^L.
>9E3 2.3E3
C"
1
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V /v \ A xv r\J\L A\ A ^/^/^A/^ ^WV /S^AA/\A A A77^4S^. \A. A^/^\
_V-/ V\^/V^A^7 M ^/W VAAf 'lA^/^W^/^ wVAA^MA^^^-VrP'll
2S.-36 28-48 29\ 00 29\ 12 29\ 24 29.-36 29^-48 30\00 30\12 30.-24 3fll-36 30-48 31 1- 00 31\ 12 31:2
'.1 . 9E3
'.1 . 4E3
.9 . 3E2
_4. 7E2
4 Time
File:T981957 #1-720 Acq: 18-APR-1998 06:12:52 EI+ Voltage SIS 70T Noise: 4 8
367.8949 F:2 BSUB(256, 30, -3 . 0 ) PKH(7, 5, 3, 0. 05%, 192. 0, 1 . 00%,F, T) Exp:NDB5US
TRIANGLE LABS Text :Jf23-I-3 TLIH45399 INJ. TIME - 06:13
1004
80J
60.
40.
20:
0.
Al . 73E6
ft
/ jb.81JB5
5.5E5
.4.4E5
.3.3E5
-2.2E5
'.1.1E5
fl.OFO
28:36 28':48 29\ 00 29': 12 291-24 29:36 29:48 30-00 30-12 30l-24 3ol-36 30l-48 ' 31 1- 00 ' 31s 12' 31 :24 Time
File:T981957 #1-720 Acq:18-APR-1998 06:12:52 EI+ Voltage SIR 70T Noise: 52
369.8919 F:2 BSUB(256 , 30, -3 . 0 ) PKD( 7, 5,3, 0 . OS\,208. 0, 1 . 00\,r, T) Exp-.NDBSUS
TRIANGLE LABS Text:M23-I-3 TLIH45399 IWJ. TIME = OS.-13
1003
80_
60_
40_
20_
0_
A1.15E6
•
/ A1.20£5
', y V/\^
3.6E5
.2.9£5
.2.2£5
L1.5E5
.7.3^4
28:36 281-48 2S-00 29\12 2S.-24 2S-36 2S.-48 30.' 00 30:12 3ol-24 3b.-36 30:48 ' 31 .' 00 ' 31 ',12 ' 31 1-24 Time
File:T981957 #1-720 Acq:18-APR-199S 06:12:52 EH- Voltage SIR 70T
330.9792 F:2 ExpsNDBSUS
TRIANGLE LABS Tsit:M23-I-3 TLI#45399 INJ. TIME - 06-13
1003
80.
60.
40.
20.
0.
*^*~
^28^5 ^ZijjOJ-^^v^O^^^ 25!« 29-'55 30:18 jfl.Ji JD.4J ,f.,f 3i ^ ^1.6E6
~* so
»
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-1.3JET6
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.6.5ES
.3.2E5
28:36 2fl:-48 25.-00 29-12 29':24 29:36 25>J<8 JO.' 00 30:12 3b':24 30- 36 30.' 4fl' 31:00' 31:12' 31.':24 Time
141
-------
ile:T581557 #1-425 Acq:18-APR-1998 06:12:52 EH- Voltage SIX JOT Noise-.107
73.8208 Fs3 BSUB(256, 30, -3.0) PKD(7, 5,3,0.05\,428.0,1.00\,F,T) Exp:NDB5US
TRIANGLE LABS Text:M23-I-3 TLI#45399 INJ. TIME - 06:13
File:T981957 #1-425 Acq:18-APR-1998 06:12:52 EI+ Voltage SIS 70T Noiae:88
375.8178 F:3 BSUB(256,30,-3.0) PKD(7, 5,3,0. 05\, 352.0,1.00\,F,T) Exp:NDBSUS
TRIANGLE LABS Text:M23-I-3 TLI#45399 INJ. TIME - 06:13
1003) A4.50E3 A3.70E3
31:48 32:00 32:12 32:24 32:36 32:48 33:00 33il2 33:24 33:36 33:48 34:00 34:12 34:24 34:36 34 48 Time
,.1.6E3
31:48 32:00 32:12 32:24 32:36 32:48 33:00 33:12 33:24 33:36 33:48 34:00 34:12 34:24 34:36 34 48 Time
File:T981957 #1-425 Acq:18-APK-1998 06:12:52 EI+ Voltage SIR 70T Noise:61
383.8639 F:3 BSUB( 256, 30,-3 . 0 ) PKD(7,5,3,0.05*,244.0,1.00*,F,T) Exp:NDB5US
TRIANGLE LABS Text:M23-I-3 TLI#4S399 INJ. TIME - 06:13
100$ A1.23E6
80:
60:
40:
20:
Al.09E6
A7.11E5
_ 3 . 7E5
.3.0E5
.2.2E5
Ll.5E5
-7.4E4
O.OEO
31\48 32\00' '32\'l2 32:24 32:36 32:48 33:00 33:12 33:24 33:36 33:48 34:00 34:12 34:24 34:36 34 48 Time
File:T981957 #1-425 Acq:18-APR-1998 06:12:52 EI+ Voltage SIR 70T Noise:58
385.8610 F:3 BSUB(256,30,-3.0) PKD(7, 5,3,0.051,232.0,1.001,F,T) Exp:NDB5US
TRIANGLE LABS Text:M23-I-3 TLI#45399 INJ. TIME - 06:13
1001 A2.43E6 .... ^7.5E5
80J
601
40:
201
A2.12E6
A1.41E6
I i i i i i i | i i i i i I i i i i i I i i i i i I' i i i' i i i i i I i i I i i i i i '| i i i ni | I i i i i i | i i i f i | i i il I | i i i i i |
31:48 32:00 32:12 32:24 32:36 32:48 33:00 33:12 33:24 33:36 33:48 34:00 34:12 34:24 34:36 34
.6.0E5
-4.5E5
.3 . OE5
.1. 5E5
.O.OEO
4 8 Time
File:T981957 #1-425 Acq: 18-APR-1998 06:12:52 EI+ Voltage SIR 70T
392.9760 F:3 Exp:NDB5US
TRIANGLE LABS Text:M23-I-3 TLI#45399 INJ. TIME
32:2a 32:4632:57
06:13
100J
aol
60;
40:
20:
o:
33:15
.7.5E5
.6.0E5
-4.5E5
-3.0E5
-1.5E5
31:48 32:00 32:12 32:24 32:36 32:48 33:00 33:12 33:24 33:36 33:48 34:00 34:12 34:24 34:36 34
File:T981957 #1-425 Acq:18-APR-1998 06:12:52 EI+ Voltage SIR 70T
445.7555 F:3 Exp:NDB5OS
TRIANGLE LABS Text:M23-I-3 TLI#45399 INJ. TIME - 06:13
•.O.OEO
48 Time
31:48 32:00 32:12 32:24 32:36 32:48 33:00 33:12 33:24 33:36 33:48 34:00 34:12 34:24 34:36 34
O.OEO
48 Tim,
-------
Fi±e:t9B1957 fl-i25 Acq:lB-APR-lS9B gg.-I3.-53 EI+ Voltage SIS 709 Xoiae:125
389.8156 F:3 BSUB(256r30, -3.0) PKD(7,5,3, 0. 05%,500. 0,1.00*,F,T) ExpsODSSUS
TRIANGLE LABS Text:M23-I-3 TLI#45399 JWJ. TIME - 06:13
100*
32:24 32:36 32:48 33:00 33': 12 33:24 33:36 33:48 34:00
File:T981957 #1-425 Acq:18-APR-1998 06:12:52 EI+ Voltage SIX 70T Noise:98
391.8127 F:3 BSUB(256,30r-3.0) PKD(7,5,3, 0.05%, 392. 0,1.00\,F,T) Exp:NDB5US
TRIANGLE LABS Text:M23-I-3 TLI#45399 INJ. TIME - 06:13
1004
34:12
O.OEO
34:24 Tims
1. 6E3
32:24 32:36 32:48 33:00 33':12 33:24 33:36 33:48 34':00
File:T981957 #1-425 Acq:18-APR-1998 06:12:52 EI+ Voltage SIR 70T Noise:117
401.8558 F:3 BSUB(256, 30,-3.0 ) PJO3( 7, 5, 3, 0 . 05%, 468. 0, 1. 00\,F, T) Exp:NDB5US
TRIANGLE LABS Text:M23-I-3 TLI#45399 IJKT. TIME = 06:13
1003; A1.42E6 A1.51E6
60.
40.
20.
34:12 34:24
OEO
Time
r-4.3E5
13.5E5
-2.6ES
.1. 7E5
. 8. 6E4
32:24 32':36 32:48 33:00 33:12 33:24 33 36 33:48 34:00
File:T981957 #1-425 Acq:18-APR-1998 06:12:52 EI+ Voltage SIR 70T Noise:174
403.8529 F:3 BSCTB(256, 30, -3 . 0) PKD(7, 5, 3 , 0.051, 696. 0, 1.00\,F,T) Exp:tTDB5US
TRIANGLE LABS Text:M23-I-3 TLI#45399 JWJ. TIME = 06:13
A1.17E6 A1.25E6
80J
so:
40:
20:
I I i i i i i I
34:12 34:
F 0 . OEO
24 Time
^
r.3.5E5
.2.8E5
-2.1E5
.1.4E5
-7.0E4
'34': 60'
34:13 34:22
32:24 32:36 32':48 33:00 33:12 33:24 33 36 33:48
File:T9819S7 #1-425 Acq: 18-APR-1998 06:12:52 EI+ Voltage SIR 70T
392.9760 F:3 Exp:NDB5US
TRIANGLE LABS Text:M23-I-3 TLH45399 INJ. TIME - OS.-1J
1003; . 32:28 32:46 32:57 33.1S
' ^^i^^_33:57
80J
so:
40:
20:
o.
.OEO
"l I I I I I 'I I I
34:12 34:24 Time
n7.5£5
.6. OE5
-4.5E5
.3.0E5
.1 . 5E5
3224
3236 32:48 33:00 33J2
O.OEO
33:36 33:48 34:00 34:12 34:24 Time
143
-------
'ileiTS81957 #1-629 Acq:18-APR-1998 06:12:52 EH- Voltage SIS JOT Koif»t83
407.7818 F:4 BSUB(256,30,-3.0) PKD(7, 5,3,0.05\,332.0,1.00\,F,T) Exp:NDB5US
TRIANGLE LABS Teit:M23-I-3 TLIf45399 IJTJ. TIME - 06113
1003, A3.3J.E3
35:48 36:00 36:12 36:24 36:36 36:48 37:00 37:12 37:24
File:T9819S7 #1-629 Acq:18-APR-1998 06:12:52 EI+ Voltage SIS 70T Noise:50
409.7789 F:4 BSVB(256,30,-3.0) PKD(7, 5,3,0.051,200.0,1,00\,F,T) EzpiNDBSUS
TRIANGLE LABS Teit:M23-I-3 TLI#45399 INJ. TIME - 06:13
1001
ao:
35:48 36:00 36:12 36:24 36:36 36:48 37:00 37:12
F±le:T981957 #1-629 Acq:18-APR-1998 06:12:52 EI+ Voltage SIR 70T Noise:94
417.8253 F:4 BSUB(256,30, -3. 0) PKD(7, 5,3, 0. 051,376. 0,1. 00%,F, T) Exp-.NVBSUS
TRIANGLE LABS Text:M23-I-3 TLI#45399 INJ. TIME = 06:13
A1.72E3 hA.380.93
.20E3 A A i kin .16E3
37:36
.O.OEO
37:48 Tims
37:24
37:36
1003
80:
60.
401
20:
ol
A6.13E5
A2.94E5
O.OEO
37:48 Time
_1.7E5
L1.4E5
_1.OE5
.6.8E4
-3.4E4
35:48 36:00 36:12 36:24 36:36 36:48 37:00 37:12 37:24
File:T981957 #1-629 Acq:18-APR-1998 06:12:52 EI+ Voltage SIR 70T Noise: 77
419.8220 F:4 BSUB(256, 30,-3 .0 ) PKD( 7,5, 3, 0. 05%, 308. 0,1. 00*, F, T) EJCp:NJDB5US
TRIANGLE LABS Text:M23-I-3 TLI#45399 INJ. TIME - 06:13
1004 A1.42E6
aol
37:36
.O.OEO
37:48 Time
601
401
201
Oj
A7.06E5
35:48 36(:6o' ' '36\12 ' ' 36\ 24 ' ' 36*:36 ' ' 36\46 ' ' 37:6o' ' ' 37\ 12
File:T981957 #1-629 Acq:18-APR-1998 06:12:52 EH- Voltage SIR 70T
430.9729 F:4 Exp:m>B5US
TRIANGLE LABS Tejct:M23-I-3 TLI#45399 INJ~. TIME
36:41 36:53 37:06
3.51:5
.3.1E5
.2.3E5
.1.6E5
.7.8E4
T—I—r=r^T""r I I I i I
37:24 37:36
'37\48
O.OEO
Tine
06:13
80:
60:
401
201
0.
37:32
-5.4E5
--4.4E5
-3.3E5
-2.2E5
.1.1E5
T~
rr
-r
35:48 36:00 36:12 36': 24 36:36 36':48 37:00
File:T981957 #1-629 Acq:18-APR-1998 06:12:52 EI+ Voltage SIR TOT
479.7165 F:4 Exp:NDB5US
TRIANGLE LABS Teit:M23-I-3 TLI#45399 INJ. TIME
' 37\24
O.OEO
37:36
~J7:48 Time
1001
36:12
06:13
36:31
35:48
36:00
36:12
36:24
36:36
36:48
37:00
37:12
37:24
37:36
O.OEO
37:48 Time
144
-------
Fi±e:t9B1957 #1-629 Acq:lB-ApR-199B 06:12:52 gl+ Voltage SIR 709 Hoime:Sl
423.7766 F:4 BSUB(256,30, -3.0) PXD(7,5,3,0. 05\,204. 0,1.00*,T,T) ExpsSDBSVS
TRIANGLE LABS Tsxt:M23-I-3 TLI#45399 IKJ. TIME - 06il3
1003> • A2.65E3
80.
36:00 36:06 36:12 36:18 36:24 36:30 36:36 36:42 36:48 36:54 J7.-00 37:06 37:12 37:ia'
File:T981957 #1-629 Acq:18-APS-1998 06:12:52 EI+ Voltage SIS 70T Noise:56
425. 7737 F:4 BSUB(256,30,-3.0) PKD(7,5,3,0.051,224.0,1.00\,F,T) ExpsNDBSOS
TRIANGLE LABS Text:M23-I-3 TLI#45399 INJ. TIME - 06:13
100$ A1.54E3
O.OEO
Time
36:00 36:06 36:12 36:18 36:24 36:30 36:36 36:42 36':48 36:54 37:00 37:06 37:12 37:18
File:T981957 #1-629 Acq: 18-APR-1998 06:12:52 EI+ Voltage SIR 70T Noise: 76
435.8169 F:4 BSUB(256, 30,-3 . 0) PKD( 7, 5, 3, 0 . 05%, 304. 0, 1. 00%,f, T) Exp-.NDBSUS
TRIANGLE LABS Text:M23-I-3 TLI#45399 INJ. TIME = 06:13
A8.50E5
BO:
so:
40:
20:
~r
~r
-r
~r
rr
~r
T
36:00 36:06 36:12 36:18 36':24 36:30 36:36 36:42 36:48 36:54 37:00 37:06 37': 12 37': 18
File:T981957 #1-629 Acq:18-APR-1998 06:12:52 EI+ Voltage SIR 70T Noiae:73
437.8140 F:4 BSUB(256, 30, -3 . 0) PKD( 7, 5,3, 0. 051,292. 0, 1. 00%,F, T) Exp:NDB5US
TRIANGLE LABS Text:M23-I-3 TLI#45399 INJ. TIME - 06:13
1003, A8.34E5
801
60.
40.
20.
o:
36:00 36:06 36:12 36:18 36:24 36:30 36:36 36:42 36:48 36:54
Tile:T9819S7 #1-629 Acq:18-APR-1998 06:12:52 EI+ Voltage SIR 70T
430.9729 F:4 Exp:NDB5VS
TRIANGLE LABS Text:M23-I-3 TLI#45399 INJ. TIME - 06:13
36:53 37:01 37±06_
37:00 37:06 37:12 37:18
O.OEO
Time
2.2E5
1.8E5
1.3E5
8. 8E4
4.4E4
.O.OEO
Time
.2.1E5
.1. 7E5
.1.2E5
.8.3E4
.4.2E4
.O.OEO
Time
801
601
401
201
01
36:bb'
4.4E5
3.3E5
2.2S5
O.OEO
Tim,
-------
rile:T9819S7 #1-629 Aci»-»ii •-! « *-«fkf^ i-*~*-i^ii^i ft. r*i n^^-.^ ri.fAn-jr~»_-fii-r~,-Lr -
40:00 41:00 42:00
SIR 70T
INJ-. TIME =06:13
27 40:33 41:14 41:42 42:39
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INJ. TIME - 06:13
39:46
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'*^^rt*'^/^^^lM*<'^^^VV'^l>^*^*^^^
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.2.114
L1.9E4
.1 . 7E4
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_1 . 3£4
_1 . 11J4
_8.4E3
-6.3E3
-4.2E3
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TjJte
_1 . 6E4
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_1.1E4
_9 . 5E3
_7.9E3
_6.3E3
_4.8£3
_3.2£3
.1.6E3
Time
5.5E5
.4.9Z5
.4.4E5
.3 . 8E5
.3.3E5
.2.7E5
.2.2E5
.1.6E5
.1 . 1E5
.5.5E4
'• 0 . OEO
Time
4.3E3
.3.9E3
.3 . 4E3
-3.0E3
.2.6E3
.2.2E3
.1 . 7E3
-1.3E3
-8.6E2
45F3
. Jf ^
: 0 . OEO
Time
146
-------
File:T9Bl957 il-629 Acq:lB-APR-1996 06:12:52 E1+ Voltage SIS 70t Noiee:4B
457.7377 T;4 BSUB(256, 30, -3. 0) PKD(7, 5,3, 0. 05%, 192. 0, 1. 00\,F, T) Exp:NDB5US
TRIANGLE LABS Text:M23-I-3 TLI#4S399 TJKJ. TIME * 06:13
1004 A5.62E3
ao:
60.
40.
20.
T
~r
T
40:18 40:24 40:30 40:36 40:42
rile:T981957 #1-629 Acq:18-APR-1998 06:12:52 EI+ Voltage SIS 701 Noise:59
459.7348 F:4 BSUB(256,30,-3.0) PXD(7,S,3, 0. 05\,236. 0,1.00\,F,T) ExpsSDBSUS
TRIANGLE LABS Teit:M23-I-3 TLI#45399 my. TIME - 06:13
1001 A2.18E3
BO.
60.
40.
20.
40:48
40:18 ~40':24'40:30 4o':36' 40:42
File:T981957 #1-629 Acq:18-APR-1998 06:12:52 EI+ Voltage SIR 70T Noise:81
469.7779 F:4 BSUB(256,30,-3 .0) PKD(7, 5, 3, 0. 05\,324 . 0, 1. 00\,F, T) Elp:NDB5US
TRIANGLE LABS Text:M23-I-3 TLI#45399 INJ. TIME = 06:13
100$ A6J3E5
1 1 •"
40:48
80.
50.
40.
20.
40:18 40:24 40:30 40.-36 ' ' ' 40j42 ' ' ' 40:40'
File:T981957 #1-629 Acq: 18-APR-1998 06:12:52 EH- Voltage SIR 70T Noise:53
471.7750 F:4 BSUB(256, 30, -3 . 0) PKD(7, 5, 3, 0 . 051,212. 0, 1. 00*,F,T) Exp:NDB5US
TRIANGLE LABS Text:M23-I-3 TLI#45399 INJ. TIME = 06:13
1003
80.
60.
40.
20.
A7.
40:18 40:24 40:30 40:36
F±le:T981957 #1-629 Acq:18-APR-1998 06:12:52 EH- Voltage SIR 70T
430.9729 F:4 Exp:NDB5OS
TRIANGLE LABS Teit:M23-I-3 TLI#45399 INJ. TIME
40:42
40:48
.9.6E2
.7.7E2
.5.8E2
.3. 8E2
.1.9E2
O.OEO
Tine
.7.5E2
.6.0E2
.4.5E2
.3. OE2
.1.5E2
.O.OEO
Time
.1. 3E5
.1. 1E5
.7.9E4
.5.3E4
.2.6E4
.O.OEO
Time
.1. 5E5
.1. 2E5
.9.0E4
.6.0E4
.3.0E4
.O.OEO
Time
06:13
J.UU3
80.
60.
40.
20.
0.
40±23 40i3J 40:38
401-18 401-24 401-30 40.-36 401-42 ' ' ' 401-48 ' ' '
5.5£5
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-3.3E5
.2.2ES
.1.1E5
0 OEO
Time
-------
Channel I 338,9798 Peak top
Helott ,78 volts Span 288 pc*
Systei file naee
Data file naae
Resolution
Group nuiber
Icnlzatlon icde
Switching
fcesus
fl=T381948
2
El*
VOLTflGE
lasses 232,9825, 416,$
R 283 J 331 32
K 332
I 334
ft 348
H 342
0 352
P 354
9 356
8 384
C 386
D 316
E 318
F 328
6 322
H 328
T 378
U 376
V 418
331 R
Ref.'iass 416,3768 Peak top
Height ,17 volts Span 288 ppi
J48
-------
23:00 24:00 25:00
File:T981957 #1-720 Acq:18-APR-1998 06:12:52 EI+ Voltage SIR 70T
305.8987 F:2 Exp:NDB5US
Sample Text:M23-I-3 TLI#45399 INJ. TIME = 06:13 File Text:M23-I-
100%
Pile:T981957 #1-720 Acq:18-APR-1998 06:12:52 EI+ Voltage SIR VUT
303.9016 F:2 Exp:NDB5US
Sample Text:M23-I-3 TLIt45399 INJ. TIME = 06:13 File Text:M23-I-
100*
3 TLI#»
_4.1E3
.O.OEO
Time
3 TLI#»
^5.8E3
0
25:00
23:00 24:00
File:T981957 #1-720 Acq:18-APR-1998 06:12:52 EI+ Voltage SIR 70T
315.9419 F:2 Exp:NDB5US
Sample Text:M23-I-3 TLI#45399 INJ. TIME = 06:13 File
100%
80 j
60 J
401
20J
Text:M23-I-
25:24
23:00
24100
LO.OEO
Time
3 TLI#»
6.8E5
L5.5E5
_4.1E5
_2.7E5
_1.4E5
25:00
O.OEO
Time
-------
Pile;T981957 #1-629 Acq;18-APR-1998 06:12:52 EI+ Voltage SIR 70T
457.7377 F:4 Exp:NDB5US
Sample Text:M23-I-3 TLI#45399 INJ. TIME =
100% A3.26E3
80 j
60J
40J
20J
39:00 40:00 41:00
File:T981957 #1-629 Acq:18-APR-1998 06:12:52 EI+ Voltage SIR 70T
459.7348 F:4 Exp:NDB5US
Sample Text:M23-I-3 TLI#45399 INJ. TIME =
100%
80J
60J
40J
20 J
06:13 File Text:M23-I-3 TLI#»
1.3E3
L1.1E3
L8.0E2
L5.3E2
L2.7E2
LO.OEO
Time
42:00
06:13 File Text:M23-I-3 TLI#»
1.7E3
L1.4E3
L1.0E3
16.9E2
L3 . 5E2^
LO.OEO
39:00 ' 40:00 41:00
File:T981957 #1-629 Acq:18-APR-1998 06:12:52 EI+ Voltage SIR 70T
469.7779 F:4 Exp:NDB5US
Sample Text:M23-I-3 TLI#45399 INJ. TIME =
100%
80 j
60 J
40 j
20 J
42:00
Time
39:00
4o!oo
06:13 File Text:M23-I-3 TLI#»
1.3E5
Ll.lES
L7.9E4
L5.3E4
L2.6E4
O.OEO
41:00
42:00
Time
-------
TLI Project: 45399
Client Sample: M23-I-3
Method 23 TCDD/TCDF Analysis (DB-225)
Analysis File: P981308
Client Project:
Sample Matrix:
TLI ID:
Sample Size:
Dry Weight:
GC Column:
r012.002/Lime Kiln
M23
204-92-3A-D
1.000
n/a
DB-225
Date Received:
Date Extracted:
Date Analyzed:
Dilution Factor:
Blank File:
Analyst:
04/01/98
04/03/98
04/16/98
n/a
U980780
ML
Spike File:
ICal:
ConCal:
% Moisture:
% Lipid:
% Solids:
SPC2NF04
PF24098
P981302
n/a
n/a
n/a
Analytes
Amt (
n«j) BTA
jEMPO -- --
fcafc
1ft Ffege
2,3,7,8-TCDF
13C12-2,3,7,8-TCDF
EMPC
0.007
3.2
79.7
40%-130%
0.77
22:24
JB_
• Internal Standard ..V.ov^.v.v
Amti ;i[rig)
% Recovery
OC Limits
Ratio
fit
Ffegs
Recovery Standard
Ratio
ITF
13C,:-1,2,3,4-TCDD
0.81
21:17
Data Reviewer.
04/20/98
Page 1 of 1
C2NFJ>SR V2.02, LARS 6.H M
Triangle Laboratories, Inc.®
801 Capitola Drive • Durham, North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 21:30 04/20/98
1 ^
-------
Data Review By:
Initial Date...
'J <^,w
Calculated Noise Area:
0.12
The Total Area for each peak with an ion abundance ratio outside
ratio limits has been recalculated according to method requirements.
Page No.
04/20/98
Listing of P981308B.dbf
Hatched GC Peaks / Ratio / Ret. Time
Compound/
M_Z.... QC.Log Omit Why ..RT. OK Ratio Total.Area... Area.Peak. 1.. Area.Peak.2. . Rel.RT Compound.Name.. ID.. Flags.
TCDF
304-306
304-306
13C12-TCDF
316-318
316-318
13C12-TCDD
332-334
332-334
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
0.
NL 0:00 RO
SN 17:51
18:52
SN 19:06 RO
SN 19:44 RO
20:01 RO
20:33
SN 20:39
21:00
SN 21:15 RO
SN 21:28 RO
22:26 RO
SN 22:39 RO
23:05
SN 23:50 RO
6 Peaks
0,
NL 0:00 RO
WL 20:59
22:24
23:04
WH 23:28 RO
WH 24:25
2 Peaks
0
NL 0:00 RO
19:54
21:01
21:17
22:01
4 Peaks
65-0.89
1.17
0.86
0.65
0.45
0.15
0.42
0.77
0.73
0.69
0.44
0.56
0.63
0.27
0.85
1.10
,65-0.89
1.00
0.78
0.77
0.81
3.64
0.83
.65-0.89
1.25
0.74
0.79
0.81
0.78
0.11
0.13
0.51 0.20
0.23
0.07
0.37 0.16
0.55 0.24
0.26
0.76 0.31
0.28
0.21
0.67 0.29
0.07
0.48 0.22
0.18
3.34
0.14
1.05
400.68 174.26
0.65 0.29
0.50
5.22
401.33
Above: TCDF / TCDD Follows -
0.14
0.61
287.19
373.95
2.15
663.90
0.26
126.85
167.21
0.94
0.790-1.102
0.000
0.797
0.31 0.842
0.853
0.881
0.38 0.894
0.31 0.917
'0.922
0.45 0.938
0.949
0.958
0.46 1.001 2378-TCDF
1.011
0.26 1.031
1.064
0.955-1.045
0.000
0.937
226.42 1.000 13C12-2378-TCDF ISO
J
J
AN J
0.36
1.030
1.048
1.090
0.905-1.095
0.000
0.35 0.947
160.34 1.000 13C12-2378-TCDD IS1
206.74 1.013 13C12-1234-TCDD RSI
1.21 1.048
Triangle Laboratories, Inc.® Analytical Services Division
801 Caprtola Drive • Durham, North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 21:30 04/20/98
15?
-------
Page No. 2 Listing of P981308B.db£
04/20/98 Matched GC Peaks / Ratio / Ret. Time
Compound/
M_Z.... QC.Log Omit Why ..RT. OK Ratio Total.Area... Area.Peak.1.. Area.Peak.2.. Rel.RT Compound. Name.. ID.. Flags.
Column Description "Why" Code Description QC Log Desc.
M_Z -Nominal Ion Mass(es) WL-Below Retention Tim* Window A-Peak Added
..RT. -Retention Time (nm:ss) HH-Above Retention Time Window K-Peak Kept
Rat.l -Ratio of M/M+2 Ions SN-Below Signal to Noise Level D-Peak Deleted
OK -RO=Ratio Outside Limits
-------
file:P9B130B #1-1006 Aoq:16-APR-lSSB 18:58:34 XI+ Voltage SIS 709
303.9016 Eip:DS225
TRIANGLE LASS Teit:H23-I-3 TLH45399
21-00 21:12 21:24 21:36 21:48 22:00 22:12 22:24 22:36 22:48 23:00 23:12 23:24
File:P981308 01-1006 Acq:16-APK-1998 18:58:34 EI+ Voltage SIR 70P
315.9419 Exp:DB225
TRIANGLE LABS Text:M23-I-3 TLI#45399
1004
95.
SO.
85J
flOJ
75j
70:
60l
55.
50.
40.
35.
30l
25.
30.
101
5j
OJ
22; 24
23:36 23:48 24 00 Tine
-4.1E5
~-3. 9E5
L 3. 7E5
L3. 5E5
L3.3E5
'-3.1E5
L2.9E5
'-2.7ES
L2.5E5
.2. 3E5
-2.0ES
.1. 8E5
_1. 6E5
.1. 4E5
-1.2ES
.1. OE5
.8.2E4
.6.1E4
.4.1E4
-2.0E4
'
21 O212 2l242136 21:48 ' 22\ 00 ' 22: 12 23\24 23t3
-------
file,P98130B tl-1006 Acq,16-APR-1998 18:58:34 EI+ Voltage SIS 7OP thime,37
303.9016 BSUB(256,30,-3.0) PKD(5, 3,1, 0.10\, 148.0,0. 00\,r,F) Sxp,DB225
TRIANGLE LABS Text,M23-I-3 TLIt45399
1003k
18:00 19:00 ' 20:00 21:00 22:00 23:00
File:P981308 tl-1006 Acq: 16-APR-199B 18:58:34 EI+ Voltage SIX TOP Noise:32
305.8987 BSUB(256,30,-3.0) PKD(S,3rl,0.10\,128.0,0.00\,F,F) Sip:DB225
TRIANGLE LABS Teit:M23-I-3 TLI*45399
A4.45E3
24:00
25:00
OEO
Tims
18:00 19:00 20-00 21:00 22:00 23:00
F±le:P981308 #1-1006 Acq:16-APR-1998 18:58:34 EI+ Voltage SIR 70P Noiae:42
315.9419 BSUB(256,30,-3.0) PKD(5, 3,1, 0.10%, 168. 0, 0. 00%,F,F) Eip:DB225
TRIANGLE LABS Tezt:M23-I-3 TLI#45399
10 03, A1.74E6
80.
60.
40.
20.
0.
24:00
25:00
rr
T
18:00 15:00 20iOO 21:00 22:00 23:00
F±le:P9S1308 tl-1006 Acq>16rAPR-199B 18:58:34 EI+ Voltage SIS 70P Noise:38
317.9389 BSUB(256,30,-3.0) PKD(5, 3,1, 0.101,152.0,0.00*,F,F) Exp:DB225
TRIANGLE LABS TextiM23-I-3 TLI#45399
24 • 00
1003
flOJ
60.
40.
20:
A2.26E6
25:00
rs.
.4.
.3.
.2.
.1.
~r
-r
T
T
18:00 15:00 201-00 21.-00 22:00 23:00
File:P981308 #1-1006 Acq:16-APR-1998 18:58:34 EI+ Voltage SIR 70P
375.8364 Ezp:DB225
TRIANGLE LABS Text:M23-I-3 TLI#45399
i i |—i—
24:00
1001
80.
60.
40.
20.
0.
17:56
""—'—'—t
25:00
2.
.1.
.1.
.9.
33,35
24:25
,
*^
18,00
19,00
20,00
21:00
22; 00
23*00
24>00
OEO
Time
1E5
3E5
5E5
6E5
2E4
OEO
Time
2E5
1E5
1E5
1E5
OE5
OEO
Time
4E3
9E3
4E3
6E2
8E2
OEO
Time
-------
'ile:PSB130B #1-1006 Acqil6-APX-1998 1U:5B:34 EI+ Voltage SIS 70P Noise:40
319.8965 BSUB(256,30,-3.0) PKH(5,3,1, 0.10\, 160.0,0.00\,F,F) ExpsDB225
TRIANGLE LASS TextsM23-I-3 TLIt45399
1004
19:00 20:00 21:00 22': 00 23': 00
F±le:P981308 #1-1005 Aoq:16-APR-1998 18:58:34 gl+ Voltage SIR TOP No±*e>38
321.8936 SSUS(256,30,-3.0) PKD(5,3,1,0.10\,1S2.0,0.00\,F,F) Eip:DB225
TRIANGLE LABS Text:M23-I-3 TLH45399
100
19:00 ' 20:00 21:00 22:00 23:00
File:P981308 #1-1006 Acq:16-APR-1998 18:58:34 EI+ Voltage SIR 70P Noiae:40
327.8847 BSVB(256,30,-3.0) PKD(5, 3,1, 0.10\,160. 0,0. 00%,F,F) Exp:DB225
TKIANGLE LABS Text:M23-I-3 TLI#4S399
1004 A2.Q4E6
80.
60.
40.
20.
19:00 20:00 21:00 22:00 23:00
File.-PS81308 #1-1006 Acq:16-APR-1998 18:58:34 EH- Voltage SIR 70P Koise:50
331.9368 BSUB(256,30,-3.0) PKD(5, 3,1, 0.10\,200. 0,0.00\,F,T) Exp:DB225
TRIANGLE LABS Teit:M23-I-3 TLI#45399
100* A1.67E6
so:
60.
40:
20.
A1.27E6
19:00 20:00 21:00 22:00 23:00
Fd.le:P981308 #1-1006 Acqtl6-APR-1998 18:58:34 EI+ Voltage SIR 70P Noiae:41
333.9338 BSUB(256,30,-3.0) PJCDf 5, 3,1, 0.10\, 164.0,0.00\,F,F) Exp:DB225
TRIANGLE LABS Text:H23-I-3 TLI#45399
1001
80.
60.
40.
SOI
0.
Al.60X6
19:00
20100
21:00
22:00
24:00
24 : 00
24: 00
24:00
6.7E5
.5.3E5
'.4.-OE5
.2.7E5
.1.3E5
O.OEO
Time
.3. 5E5
.2.6E5
.1. 7E5
.8.7E4
O.OEO
Time
-4.2E5
.3.1E5
.2.1E5
.1. OE5
23100
24:00
O.OEO
Tims
-------
rileiP981308 #1-1006 Acqsl6-APR-1998 18,58:34 EI+ Voltage SIS 7OP
303.9016 Exp:DB225
TRIANGLE LABS Teit:H23-I-3 TLH45399
10:00 19:00 20:00 21:00
File:P98130e #1-1006 Acq:16'-APK-1998 18:58:34 XI+
315.9419 Exp:DB225
TRIANGLE LABS Text:H23-I-3 , TLH45399
100*
80
sol
40:
20:
ol
22:00 23:00 24:00
Voltage SIR 7OP
22:24
25100
22:00 ' 23:00
18:00 15:00 20:00 21:00
file:P981308 #1-1006 Acq:16-APR-1998 18:58:34 EI+ Voltage SIS 70P
319.8965 Exp:DB225
TRIANGLE LABS Text:M23-I-3 TLI#45399
—i—I—i—r
24:00
100J
80:
60:
40:
201
ol
18:42
25
25:00
~r
~r
21:01
18:00 IPiOO 20 .-00 211-00
ttletP981308 #1-1006 Acq:16-APR-1998 18:58:34 EI+
331.9368 Eip:DB225
TRIANGLE LABS Teit:M23-I-3 TLI#4S399
1003t 21
80j
60l
401
20:
0.
22:00 2JiOO
Voltage SIR 70P
24-00
25 i
4.
'•.3.
12.
.1.
.8.
18:00 19:00 201-00 21:00
file:P981308 #1-1006 Acg.-16-APB-1998 18:58:34 EI+
292.9825 Exp:DB225
TRIANGLE LABS Teit:M23-I-3 TLI#45399
1003, 18:42 19:28 19:57 20:57
80J
60:
40J
20J
22:00 23:00
Voltage SIS 70P
'.i3p 21:59 22:43 23:25
24 • 00
~"—'—I
25:00
24:41
18:00 19:00 20:00 21:00
File:P981308 #1-1006 Acq:16-APR-1998 18:58:34 EI+
330.9792 ExpiDB225
TRIANGLE LABS Text:M23-I-3 TLI#45399
22:00 23:00
Voltage SIS 7OP
i I—i—r-
24:00
25:
1001
80:
60:
40:
20:
ol
18:19
19:36
21:29 _ 22:1322:40 23:15 23:51 24:23
18:00
15:00
20:00
21:00
22:00'23-00 '24:00
0.
:00
OEO
Time
.1E5
3JT5
5E5
6E5
2E4
.OEO
Time
1E3
1E2
8E2
.5E2
.3E2
.OEO
Time
.4E5
.5E5
.6E5
.7E5
.7E4
.OEO
Time
.2E6
.6ES
.2E5
.8ES
.4E5
,OEO
Time
5E6
2E6
7E5
8E5
9E5
OEO
Time
-------
56
fl:P981388
Ref, lass 292,9825 Peak top
Heloht ,17 volts Span 288 pp
Systei file naie
Data filena*
Resolution
Group ninber
lonizatlon nde
Switching
Ref, lasses 292,9825,
fl 292,9825
B 383,9816
C 385,8987
D 315,9419
E 317,9389
F 319,8965
6 321,8936
H 327,8847
I 338,9792
j
K
L
H
1
EI+
VOLTRGE
388,9761
338,9792
331,9368
333,9338
375,8364
Channel I 338,9732 Peak top
Height ,19 volts Sp* 288 ppi
158
-------
File:P981308 #1-1006 Acq:16-APR-1998 18:58:34 EI+ Voltage SIR 70P
303.9016 Exp:DB225
Sample Text:M23-I-3 TLI#45399 File Text:M23-I-3 TLI#45399
21:00 22:00 23iOO 24:00
File:P981308 #1-1006 Acq:16-APR-1998 18:58:34 EI+ Voltage SIR 70P
305.8987 Exp:DB225
Sample Text:M23-I-3 TLI#45399 File Text:M23-I-3 TLI#45399
100%.
A4.60E3
25:00
21:00
22:00
23:00
24:00
25:00
.O.OEO
Time
-------
Pages 160 through 244 from the Triangle Laboratories, Inc. analytical report
have been excluded by PES since these pages present results for samples
collected at another lime kiln facility during the same mobilization.
-------
TLI Project: 45399
Client Sample: M23-O-3
Method 23 TCDD/TCDF Analysis (DB-225)
Analysis File: P981312
Client Project:
Sample Matrix:
TLI ID:
Sample Size:
Dry Weight:
GC Column:
r012.002/Lime
M23
204-92-7A-D
1.000
n/a
DB-225
Kiln
Date Received:
Date Extracted:
Date Analyzed:
Dilution Factor
Blank File:
Analyst:
04/01/98
04/03/98
04/16/98
n/a
U980780
ML
Spike File:
ICal:
ConCal:
% Moisture:
% Lipid:
% Solids:
SPC2NF04
PF24098
P981302
n/a
n/a
n/a
Anafytes
2,3,7,8-TCDF
internal Standard,
13C,r2,3,7,8-TCDF
*>* ,-'r 'Aiwt'lNfr #$f^«*i* ^ m/jsg&kg**
-'- \- % ^ , Ar
Recovery SiandardK ; '
ND 0.007
at"{'a§)""\^g;p^
2.4 60.0
- „"
iwr?' OCltmM:-
40%-130%
^V^' * ' "f
0.80
" - fMksr : "
—
»&:' Ffe^
22:24
*%r :,!**•»':
I3C12-1,2,3,4-TCDD
0.80 21:17
Data Reviewer.
Page 1 of 1
04/20/98
C2NFJ>SR TlOZ LARS 6.11.00
Triangle Laboratories, Inc.®
801 Capitola Drive • Durham, North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 21:29 04/20/98
-------
Initial
.Dace.
Data Review By:
Calculated Noise Area: 0.16
The Total Area for each peak with an ion abundance ratio outside
ratio limits has been recalculated according to method requirements.
Page No.
04/20/98
Listing of P981312B.dbf
Hatched GC Peaks / Ratio
/ Ret. Time
Compound/
M_Z QC.Log Omit Why ..RT. OK Ratio Total.Area... Area.Peak.1.. Area.Peak.2.. Rel.RT Compound.
ID.. Flags.
TCDF
304-306
304-306
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
NL
SN
SN
SN
SN
SN
SN
SN
SN
SN
SN
SN
0
0
18
18
19
20
:00
:43
:52
:09
:03
20:33
20
22
23
23
23
23
:59
:26
:05
:37
:41
:45
0.
RO
RO
RO
RO
RO
RO
RO
RO
RO
RO
65-0.89
0
1
0
9
1
0
1
1
0
0
0
3
.89
.00
.39
.00
.00
.43
.00
.08
.67
.29
.50
.50
Peaks
0.17
0.04
0.21
0.02
0.11
0.07
0.25
0.23
0.10
0.05
0.07
0.04
0.00
0.790-1.102
0.000
0.836
0.842
0.855
0.895
0.917
0.937
1.001 2378-TCDF
1.031
1.054
1.057
1.060
AN
13C12-TCDF
316-318
316-318
13C12-TCDD
332-334
332-334
DC
DC
DC
DC
DC
0.
NL 0:00 RO
WL 20:59
WL 21:14 RO
22:24
WH 24:26 RO
1 Peak
0
NL 0:00 RO
21:01
21:17
22:01
3 Peaks
65-0.89
1.11
0.78
1.33
0.80
0.99
.65-0.89
1.38
0.76
0.80
0.78
0.16
0.71
0.48
250.64
4.09
250.64
111.01
Above: TCDF / TCDD Follows
0.14
176.85
310.87
1.42
489.14
76.25
138.30
0.62
0.955-1.045
0.000
0.937
0.948
139.63 1.000 13C12-2378-TCDF ISO
1.091
0.905-1.095
0.000
100.60 1.000 13C12-2378-TCDD IS1
172.57 1.013 13C12-1234-TCDD RSI
0.80 1.048
Column Description 'Why Code Description QC Log Desc.
M_Z -Nominal Ion Mass(es)
. .RT. -Retention Time (nnuss)
Rat.l -Ratio of M/M+2 Ions
OK -RO-Ratio Outside Limits
Rel.RT-Relative Retention Time
*** End of Report
WL-Below Retention Time Window A-Peak Added
WH-Above Retention Time Window
SN-Below Signal to Noise Level
-------
'ile:P9ai312 #1-1006 Acq:16-APR-19ya U: 12:13 EI+ Voltage SIR 7OP B6iae:41
03.9016 BSUB(256,30,-3.0) PKD(5,3,1, 0.10\, 168.0,0.00\,r,f) Exp:DB225
TRIANGLE LABS Text:M23-O-3 TLH45399
004 A910.93
18:00 19:00 20:00 21:00 22:00 23:00
riletP981312 11-1006 Acq:16-APR-1998 22:12:13 11+ Voltage SIX 70P Ooite:44
305.8987 BSUB(256,30r-3.0) PKD(5,3,1, 0.10\, 176.0,0.00\,r,F) Exp:DB225
TRIANGLE LABS Text:H23-0-3 TLH45399
1004 A2.26X3
80.
60.
40.
20:
A1.42X3
A60S.41 A1.38E3
A334.0S
24100
18:00 19:00 20:00 21:00 22:00 23:00
TilesP981312 #1-1006 Acq:16-APR-1998 22:12:13 EI+ Voltage SIS 70P Hois*-.48
315.9419 BSUB(256,30,-3.0) PKD(5,3,1, 0.10%, 192.0,0.00\,T,T) Exp:DB225
TRIANGLE LABS Text:M23-O-3 TLI#45399
2004 A1.11E6
BO:
60:
40.
201
24:00
18:00 19:00 . 20:00 21:00 22:00 23:00
File:P981312 #1-1006 Acqsl6?APR-1998 22:12:13 EI+ Voltage SIX 70P Soiae:46
317.9389 BSUB(256,30,-3.0) PKD(5,3,l,0.10\,184.0,0.00\,r,r) Eip:DB225
TRIANGLE LABS Text:H23-O-3 TLI#4S399
1004 A1.40E6
80.
60.
40.
20.
24:00
18:00 19:00 20:00 21:00 22:00 23:00
F±le:P981312 #1-1006 Acq:16-APR-1998 22:12:13 EH- Voltage SIX 70P
375.8364 Exp:DB225
TRIANGLE LABS Text:H23-O-3 TLI#45399
1004
241 00
.5.2X2
.4.2E2
.3.1X2
.2.1E2
11. 0X2
O.OEO
25:00 Tim*
25:00 Time
,.2.6X5
'.2.1X5
_1. 6X5
.1. 1ES
.S.3E4
0.0X0
25:00 Time
.3.3E5
'.2.6X5
'.2.0E5
11.3X5
.6.5X4
O.OEO
25:00 Tic
18:00
19:00
20:00
21: 00
22 s 00
23100
24100
O.OEO
25:00 Time
247
-------
T±le:P9B13l2 #1-1006 Acq:16-APS-19SB 12:12:13 EH- Voltage SIX 7OP Itoiaei41
319.8965 BSOB(256,30r-3.0) PKD(5,3,1, 0.10\,164.0,0.00\,F,F) X*p:DB225
TRIANGLE LABS Text:M23-0-3 TLI#45399
•I 004 ,
15:00 20i00 21:00 22:00 23:00
File:P981312 #1-1006 Acq: 16-APR-1998 22:12:13 EI+ Voltage SIR 70P Koi.aa-.47
321.8936 BSOB(256,30,-3.0) PKD(5,3,lr0.10%, 188.0,0.00\,T,F) Xxp:DB225
TJtlANGLK LABS Teit:M23-0-3 TLH45399
19:00 20>00 21:00 22:00 23:00
File:P981312 #1-1006 Acq:16rAPB-1998 22:12:13 XI+ Voltage SIS 70P Noise:40
327.8847 BSUB(256,30,-3.0) PKD(5,3,1, 0.10\,160.0,0.00\,F,F) Xxp:DB225
TRIANGLE LABS Text:M23-0-3 TX.I#45399
Al. 75X6
24:00
ion.
A1.51X3
24:00
80.
60.
40.
20.
19:00 20:00 21:00 22:00 23:00
File:P981312 #1-1006 Acqsl6-APJt-1998 22:12:13 EI+ Voltage SIS 70P Noise-.56
331.9368 BSUB(2S6,30,-3.0) PKD(5,3,1, 0.10\,224.0,0.00\,T,T) Exp:DB22S
TSIANGLE LABS Teit:M23-O-3 TLI#45399
1001 A1.38E6
24:00
80.
60.
40.
20.
A7.63E5
19:00 20:00 21:00 22:00 23:00
f±le:P981312 #1-1006 Acq:16*APB-1998 22:12:13 EH- Voltage SIS 70P Noiae:40
333.9338 BSUB(256,30r-3.0) PTH(5,3,1,0.10\,160.0,0.00\,F,T) ExptDB225
TRIANGLE LABS TexttM23-O-3 TU#45399
1001 A1.73X6
24:00
80.
60.
40.
20.
0.
Al. 01JS6
19.-00
20:00
21:00
22:00
23)00
24:00
4.5X5
3.6X5
2.7X5
1.8X5
9.0X4
0.0X0
Time
.3.8X5
.3.0X5
.2.3X5
.1.5X5
.7.6X4
.0.0X0
Time
.4.8X5
.3.8X5
.2.9X5
.1.9X5
.9.5X4
.0.0X0
-------
file
303.
TXIA
1001
80J
60:
40:
20:
o:
rile
315.
TKIA
1003
BO:
60:
40:
20:
o-
rile
319.
TXIA
1001
ao:
60:
40:
20:
o-
rile
331.
TXIA
1001
80:
60:
40:
20:
0
rile
292.
TXIA
1001
80:
60:
401
201
o-
nit
330.
TXIA
1003
80:
60:
40:
20:
0
-.P981312 tl-1006 Acqil6-APX-1998 22:12:13 EH- Voltage SIS 70P
9016 Exp:DB225
tfGLE LABS Text:M23-0-3 TZIt45399
1Bi53 20:03 a0t3320:59
S**W&™^^
10:00 19:00 20:00 21:00 22:00 23:00 24:00 25:
:P981312 tl-1006 Acq:16-APX-1998 22:12:13 EI+ Voltage SIX 70P
9419 Eip:DB225 \
OGLE LABS Text:M23-O-3 TLIt45399
22:24
11
18:00 19:00 20:00 21:00 22:00 23:00 24:00 25:
-.P981312 tl-1006 Acq:16-APX-1998 22:12:13 EI+ Voltage SIR 70P
8965 Exp:DB225
OGLE LABS Tsxt:H23-0-3 TLIt45399
i6[43 iQ,13 20sil 21 01 a3'36 24:2B
^W ,
]
iaiflO 1S.-00 ' 20:00 ' 21:00 22.-00 ' ' 231-00 ' ' 24:00 ' ' 25\
•.P981312 tl-1006 Acq: 16 -APS- 199 8 22:12:13 EI+ Voltage SIR 70P
9368 Exp:DB225
KSLE LABS Text:M23-O-3 TLIt45399
21:17
: ':
, ».„!
Illl
18:00 19:00 20:00 21:00 22: 00 23:00 24:00 25.
:P981312 tl-1006 Acq:16-APX-1998 22:12:13 EI+ Voltage SIX 70P
9825 Exp:DB225
NGLE LABS Text:M23-O-3 TLIt45399
!Bi33 -19i48 20s 56 21, -24 21:50 22:45 23 -.22 11 . AT,I . , -, ^..ff
~j~,r-T^yju / ,^- -J'--«^'^j^*^^^*ft^<^hjJ^s*yV^VMK\ r^"^*^1 ' "" liV^s-i-"--jv^rA*" y\ Ai^^ nrL/'vtmK *J.*/*4:j.J 24:45
j
18:00 19:00 20:00 21:00 22:00 23:00 ' ' ' 24:00 25
IP981312 tl-1006 Aoj:16-APX-1998 22:12:13 EI+ Voltage SIB 7 OP
9792 Ezp:DB225
\SGLE LABS TeztsM23-O-3 TLH45399
f&WVf^L^y^
•
18:00 19:00 20:00 21:00 22:00 23:00 24:00 ' ' ' 25
.1.1C3
.7.9E2
.5.312
0.0£0
00 Tiae
.2.5*5
.2.1E5
.1 . 5E5
.1.1E5
.S.3E4
O.OEO
00 Time
_1 . 1E3
.6.8E2
.4.512
1.2.312
O.OEO
00 Time
3.8E5
.3 . OE5
'-.2.3E5
.1.5E5
.7.6E4
0 . OEO
00 Time
7.4E5
.5.9ES
.4.4ES
.3 . OES
.1.5*5
O.OEO
00 Time
-8.6E5
.6.9E5
.5.215
.3.4*5
.1 . 7*5
0.0*0
• 00 Time
-------
R'P981312
Kef, lass 292,9825 Peak top
Height ,11 wits Span 288 pet
Systa file naie
Data file naie
Resolution
Group nicer
lonlzatlon nde
Switching
Ref, lasses 292,9825,
1
El*
VOGE
fl 292,9885
8 383,9818
D 315,9419
E 317,9389
F 319,8965
6 321,8936
H 327,8847
338,9792
J
K
L
II
338,9792
331,9368
333,9338
375,8364
Channel I 338,9792 Peak top
Height ,15 wits ^pan 208 ppi
250
-------
TLI Project:
Client Sample:
45399
M23-O-3
Method 23 PCDD/PCDF Analysis (a)
Analysis File: S982305
Client Project:
Sample Matrix:
TLI ID:
Sample Size:
Dry Weight:
GC Column:
r012.002/Lime Kiln
M23
204-92-7A-D
1.000
n/a
DB-5
Date Received:
Date Extracted:
Date Analyzed:
Dilution Factor:
" Blank File:
Analyst:
04/01/98
04/03/98
04/18/98
n/a
U980780
DL
Spike File:
ICal:
ConCal:
% Moisture:
% Lipid:
% Solids:
SPMIT204
SF51078
S982303
n/a
n/a
n/a
Anatytes
2,3,7,8-TCDD
1,2,3,7,8-PeCDD
1,2,3,4,7,8-HxCDD
1,2,3,6,7,8-HxCDD
1,2,3,7,8,9-HxCDD
1,2,3,4,6,7,8-HpCDD
1,2,3,4,6,7,8,9-OCDD
2,3,7,8-TCDF
1,2,3,7,8-PeCDF
2,3,4,7,8-PeCDF
1,2,3,4,7,8-HxCDF
1,2,3,6,7,8-HxCDF
2,3,4,6,7,8-HxCDF
1,2,3,7,8,9-HxCDF
1,2,3,4,6,7,8-HpCDF
1,2,3,4,7,8,9-HpCDF
1,2,3,4,6,7,8,9-OCDF
:^a^p— ^'•v--r^i
Total TCDD
Total PeCDD
Total HxCDD
Total HpCDD
Total TCDF
Total PeCDF
Total HxCDF
Total HpCDF
Amt (ng)
ND
ND
ND
ND
ND
ND
ND
EMPC
ND
ND
ND
ND
ND
ND
ND
ND
ND
; ^ Amt (ngj
ND
ND
ND
ND
EMPC
ND
ND
ND
, at ; EMPO
0.006
0.009
0.01
0.01
0.009
0.01
0.02
0.007
0.006
0.006
0.006
0.006
0.007
0.008
0.01
0.01
0.01
Number DL EMPC
0.006
0.009
0.01
0.01
0.007
0.006
0.007
0.01
ffcrtH* ,8T Flag*
—
JB_
^~~~
"• fff f * j^fj-p^jL
^"|Q.Q§t
— .
Page 1 of2
Mm.PSRYl.04. LARS 6.11.00
Triangle Laboratories, Inc.*
801 Capitola Drive • Durham, North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 21:23 04/20/98
-------
TLI Project: 45399
Client Sample: M23-O-3
Method 23 PCDD/PCDF Analysis (a)
Analysis File: S982305
Internal Standards
l3C,2-2,3,7,8-TCDF
13C,2-2,3,7,8-TCDD
13C,2-l,2,3,7,8-PeCDF
13C,2-l,2,3,7,8-PeCDD
13Cp-l,2,3,6,7,8-HxCDF
I3C,2-l,2,3,6,7,8-HxCDD
13C,2-l,2,3,4,6,7,8-HpCDF
13Ci2-l,2,3,4,6,7,8-HpCDD
1SC|2-1,2,3,4,6,7,8,9-OCDD
Surrogate Standards jfType A)
'3C,2-2,3,4,7,8-PeCDF
l3C,2-l,2,3,4,7,8-HxCDF
13C,2-l,2,3,4,7,8-HxCDD
1JCi2-l,2,3,4,7,8,9-HpCDF
Other Standard
37Cl4-2,3,7,8-TCDD
Alternate Standards (Type A)
13C,2-l,2,3,7,8,9-HxCDF
13C,2-2,3,4,6,7,8-HxCDF
Recovery Standards
1JC,2-1,2,3,4-TCDD
13Ci2-l,2,3,7,8,9-HxCDD
, ' Amt (ng| ^
2.2
2.0
2.2 '
2.4
2.6
2.9
2.2
2.6
5.1
Amt. (ng)
4.1
3.9
3.9
3.8
AmL (ng)
3.9
Amt. (ng)
2.5
2.6
%^R«pw$
54.8
49.0
55.4
59.7
63.9
72.6
54.3
65.5
63.1
% Recovery
102
97.4
96.5
95.2
% Recovery
96.7
% Recovery
62.9
65.3
QC Limit*
s .. AX- A
40%-130%
40%-130%
40%-130%
40%-130%
40%-130%
40%-130%
25%-130%
25%-130%
25%-130%
QC Limits
40%-130%
40%-130%
40%- 130%
25%-130%
QCLimtts
40%-130%
QCLimtts
40%-130%
40%-130%
0.72
0.77
1.52
1.50
0.51
1.23
0.41
1.01
0.85
V *te*fc ^
1.56
0.50
1.21
0.40
._
Ratio
0.49
0.50
Ratio
0.81
1.20
^igy^ Ffepff *
25:15
25:57
29:10
30:13
32-45
33:27
35:46
36:51
40:43
8T Flags
29:52
32:39
33:23
37:22
irr „ Fia$>
25:59
IFF Flags
34:03
33:16
.8T Ftegs
25:47
33:47
Data Reviewer.
04/20/98
Page 2 of 2
MTT2JPSR »1 M. LARS 6.1140
Triangle Laboratories, Inc.®
801 Capitola Drive • Durham, North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 21:23 04/20/98
- 252
-------
Initial
Date...
Data Review By:
Calculated Noise Area:
0.19
The Total Area for each peak with an ion abundance ratio outside
ratio limits has been recalculated according to method requirements.
Page No.
04/20/98
Listing of S982305B.dbf
Hatched GC Peaks / Ratio / Ret. Time
Compound/
M_Z.... QC.Log Omit Why ..RT. OK Ratio Total.Area... Area.Peak.1.. Area.Peak.2.. Rel.RT Compound.Name.. ID.. Flags.
TCDF
304-306 AN
304-306
13C12-TCDF
316-318
316-318
37C1-TCDD
328
328
13C12-TCDD
332-334
332-334
13C12-PeCDF
352-354
352-354
13C12-PeCDD
368-370
368-370
HXCDF
374-376
DC
DC
DC
DC
DC
DC
0.
25:17 RO
1 Peak
0.
NL 0:00 RO
25:15
1 Peak
NL 0:00
24:36
25:59
2 Peaks
0.
NL 0:00 RO
25:47
25:57
26:17
3 Peaks
1
NL 0:00 RO
29:10
29:52
2 Peaks
1
NL 0:00
30:13 .
30:20
2 Peaks
1
NL 0:00
65-0.89
0.56
65-0.89
0.56
0.72
65-0.89
1.93
0.81
0.77
0.79
.32-1.78
1.00
1.52
1.56
.32-1.78
1.33
1.50
1.42
.05-1.43
1.20
0.90 0.39
0.90
0.23
380.29 158.78
380.29
0.11
2.10 2.10
239.54 239.54
241.64
0.25
483.57 216.31
261.13 113.69
3.91 1.73
748.61
TV" Fin / P^f* T\V TPrtl 1 >*\t*}a
0.12
288.35 173.76
286.96 174.74
575.31
PeCDF / PeCDD Follows — — -
0.14
172.28 103.26
15.23 8.94
187.51
•0— /*r\f\ / Hvf FM? T?rtl 1 *M*rc
0.22
0.873-1.075
0.70 1.001 2378-TCDF
0.960-1.040
0.000
221.51 1.000 13C12-2378-TCDF
0.923-1.077
0.000
0.948
1.001 37C1-TCDD
0.923-1.077
0.000
267.26 0.994 13C12-1234-TCDD
147.44 1.000 13C12-2378-TCDD
2.18 1.013
0.863-1.137
0.000
114.59 1.000 13C12-PeCDF 123
112.22 1.024 13C12-PeCDF 234
0.868-1.132
0.000
69.02 1.000 13C12-PeCDD 123
6.29 1.004
0.963-1.048
0.000
AN
ISO
CLS
RSI
I SI
IS2
SUR1
I S3
Triangle Laboratories, Inc.® Analytical Services Division
801 CapHoia Drive • Durham, North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 21:23 04/20/98
-------
Page No.
04/20/98
Listing of S982305B.dbf
Matched GC Peaks / Ratio / Ret. Time
Compound/
M_Z.... QC.Log Omit Why ..RT. OK Ratio Total.Area... Area.Peak.1.. Area.Peak.2.. Rel.RT Compound.Name.. ID.. Flags.
374-376
13C12-HxCDF
384-386
384-386
HxCDD
390-392
390-392
13C12-HXCDD
402-404
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
SN
SN
SN
SN
SN
SN
SN
SN
SN
SN
SN
0
NL
SN
SN
SN
SN
SN
SN
SN
SN
7
NL
SN
SN
SN
SN
SN
SN
SN
SN
SN
SN
WH
0
NL
31:48
31:52
32:06
32:19
32:39
32:46
32:52
33:16
33:22
34:04
34:19
Peaks
0:00
31:40
31:48
32:39
32:45
32:57
33:04
33:07
33:16
33:30
33:32
33:36
33:48
34:03
34:19
34:22
Peaks
0:00
32:39
32:44
32:52
32:58
33:08
33:13
33:24
33:29
33:43
33:48
34:02
Peaks
0:00
32:49
RO
RO
RO
RO
RO
RO
RO
RO
0.
RO
RO
RO
RO
RO
RO
RO
RO
1.
RO
RO
RO
RO
RO
RO
RO
1
RO
RO
1
4
0
1
1
1
2
2
4
1
2
.75
.00
.67
.11
.24
.26
.50
.88
.00
.44
.00
0
0
0
0
0
0
0
0
0
0
0
0
.18
.04
.07
.19
.47
.52
.09
.18
.04
.40
.09
.00
43-0.59
1
0
0
0
0
1
0
1
0
0
0
1
0
0
0
0
.14
.42
.48
.50
.51
.00
.36
.67
.50
.85
.50
.11
.93
.49
.57
.50
0
1
1
243
245
0
0
0
248
0
0
0
0
192
0
0
934
u*rr"r\
.05-1.43
0
1
0
2
1
0
1
2
1
1
1
1
.77
.80
.62
.10
.40
.75
.13
.33
.11
.00
.17
.33
0
0
0
0
0
0
0
0
0
0
0
0
0
.21
.57 0.53
.75 0.57
.29 81.15
.86 82.78
.38 0.25
.24
.14
.74 82.41
.41
.24
.14
.23
.47 63.25
.11
.12
.06
.18
.22
.14
.22
.12
.05
.32
.13
.38
.09
.26
.28
.00
.05-1.43
0
0
.67
.87
0
0
.29
.49 0.27
0
0
0
0
0
1
1
1
1
1
1
.971
.973
.980
.987
.997 123478-HxCDF
.001 123678-HXCDF
.004
.016 234678-HXCDF
.019
.040 123789-HxCDF
.048
AN
AN
AN
AN
0.878-1.122
0
1.26 0
1.18 0
162.14 0
163.08 1
0.25 1
1
1
166.33 1
1
1
1
1
129.22 1
1
1
.000
.967
.971
.997 13C12-HXCDF 478
.000 13C12-HXCDF 678
.006
.010
.011
.016 13C12-HXCDF 234
.023
.024
.026
.032
.040 13C12-HXCDF 789
.048
.049
SOR2
IS4
ALT2
ALT1
0.958-1.014
0
0
0
0
0
0
0
0
1
1
1
1
.000
.976
.979
.983
.986
.991
.993
.999 123478-HXCDD
.001 123678-HxCDD
.008
.010 1237.89-HxCDD
.017
AN
AN
AN
0.970-1.030
0
0.31 0
.000
.981
Triangle Laboratories, Inc.® Analytical Services Division
801 Caprtola Drive • Durham, North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 21:23 04/20/98
254
-------
Page No.
04/20/98
Listing of S982305B.db£
Hatched GC Peaks / Ratio / Ret. Time
Compound/
M_Z.... QC.Log Omit Why ..RT. OK Ratio Total.Area... Area.Peak.1.. Area.Peak.2.. Rel.RT Conpound.Hame.. ID.. Flags.
402-404
HpCDF
408-410
408-410
13C12-HpCDF
418-420
N
418-420
HpCDD
424-426
424-426
13C12-HpCDD
436-438
436-438
33:23
33:27
33:47
4 Peaks
DC NL 0:00
DC SN 37:36
DC WH 37:44
0 Peaks
DC NL 0:00
35:46
DC SN 36:12
37:22
2 Peaks
DC NL 0:00
DC SN 36:04
DC SN 36:16
DC SN 36:28
DC SN 36:52
DC WH 37:15
0 Peaks
DC NL 0:00
36:51
DC SN 37:09
1 Peak
0.
RO
RO
RO
0.
RO
RO
0.
RO
RO
RO
RO
RO
0
RO
1.
1.
1.
21 179.55 98.41
23 202.40 111.58
20 301.89 164.45
684.33
_ AVvftira. . Uv/TVn / Ov*S*1\O V.n.1 1 «.»
88-1.20
1.
0.
1.
45
40
33
0,
0.
0.
0.
.22
.04
.24
.00
37-0.51
1.
0.
1.
0.
33
41
29
40
0,
138,
0,
105,
244,
Lj***~m
.88-1.20
1.
0.
1.
1.
0.
0.
30
80
00
78
58
82
0,
0
0
0
0
0
0
.17
.97 40.68
.24
.98 30.53
.95
.20
.16
.04
.18
.29
.18
.00
.88-1.20
1.
1.
0.
06
01
31
0
146
0
146
.35
.39 73.47
.10
.39
81.14 0
90.82 1
137.44 1
.998 13C12-HXCDD 478 SDR3
.000 13C12-HXCDD 678 IS5
.010 13C12-HXCDD 789 RS2
0.997-1.051
0
1
1
.000
.051
.055
0.944-1.112
0
98.29 1
1
75.45 1
.000
.000 13C12-HpCDF 678 IS6
.012
.045 13C12-HpCDF 789 SUR4
0.976-1.005
0
0
0
0
1
1
.000
.979
.984
.990
.000 1234678-HpCDD AN
.011
0.973-1.027
0
72.92 1
1
.000
.000 13C12-HpCDD 678 IS7
.008
Above: HpCDD / Octa-CDD and CDF Follows
OCDF
442-444
442-444
0.76-1.02
DC NL 0:00 0.83
DC WL 36:36 RO 0.27
DC WL 36:40 RO 0.33
DC SN 36:47 RO 0.29
DC SN 37:14 RO 0.43
DC SN 37:37 RO 0.50
DC SN 38:26 RO 0.70
DC SN 38:34 RO 0.27
DC SN 42:20 RO 3.00
0 Peaks
0.22
0.13
0.06
0.11
0.19
0.11
0.30
0.06
0.06
0.00
0.902-1.098
0.000
0.899
0.901
0.903
0.914
0.924
0.944
0.947
1.040
Triangle Laboratories, Inc.® Analytical Services Division
801 Caprtola Drive • Durham, North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 21:23 04/20/98
-------
Page No.
04/20/98
Listing of S982305B.dbf
Matched OC Peaks / Ratio / Ret. Time
Compound/
M_Z QC.Log Omit Why ..RT. OK Ratio Total.Area... Area.Peak.1.. Area.Peak.2. . Rel.RT Compound.Name..
OCDD
458-460
458-460
0.76-1.02
DC NL 0:00 RO 1.29
DC SN 40:38
DC SN 40:44
DC
SN 40:50 RO
0 Peaks
1.00
0.81
0.14
0.13
0.12
0.38
0.06
0.00
0.902-1.098
0.000
0.998
1.000 OCDD
1.003
ID.. Flags.
AN
13C12-OCDD 0.76-1.02
470-472 DC NL 0:00 RO 1.38 . 0.15
40:43 0.85 191.39
DC WH 41:11 RO 0.55 0.38
470-472 1 Peak 191.39
88.03
0.996-1.004
0.000
103.36 1.000 13C12-OCDD
1.011
IS8
Column Description "Why" Code Description QC Log Desc.
M_Z -Nominal Ion Mass(es)
..RT. -Retention Time (mm:ss)
Rat.l -Ratio of M/M+2 Ions
OK -RO=Ratio Outside Limits
Rel. RT-Relative Retention Time
End of Report
WL-Below Retention Time Window
WH-Above Retention Time Window
SN-Below Signal to Noise Level
-------
JTile.-SS 02305 #1-746 Acq:18~APR-1998 11:24:51 EI+
303.9016 F:2 BSUB(256,30,
Voltage SIR 70S «toi«e:88
-3.0; PKD(9,5,5,0.05\t352.0,1.00\,r,T) Exp:NDB5US
TRIANGLE LABS Text:TLI#45399 M23-O-3
1003
80:
60:
40:
20.
0.
i 1
W*MAj^T\Ar
,J
W y\Ar
I J
u
VM
/I 1
'ulAAJ
IKT. TIME - 11:26
i
\ 1 nil
W^J^lfUJ
f.l.5E3
lsvM^v/JW^^^JiAA^^
• i-
23:00'
241-00
File:S982305 #1-746 Acq: 1B-APS-1998 11:24
305.8987 F:2 BSUB(256,30,
:51 EI+
25:00
.1.2E3
.8.8E2
.5.9E2
-2.9E2
O.OEO
26:00 27:00 ' ' Time
Voltage SIR 70S Noise -.91
-3.0; WCD(9,5,5,0.05*,364.0,1.00%,J1,T; Exp:NDB5US
TRIANGLE LABS Text:TLI#45399 M23-O-3
1003
80:
60:
40:
20:
f
,, ,. 23:
22:52 |
J__LM_I^_J
15
I
1
24
1JUAfAl '\^kjsfi 1
:15
25
24:52
i
24:33 Jt i
A iii I/1! A /
23 .-OO'
241-00 25ioO
File:S982305 #1-746 Acq:18-APR-1998
315.9419 F:2 BSUB(256,30,
-3.0; P1CD(9
11:24
,5,5,
:51 EI+
1JCJ. TIME - 11:26
16
2.4E3
25:42 26:55
jl „, 2S: 10 . 1 1 .
JtJb*\^i***j^\*^\WWvif>ff*t*A<
-2.0E3
.1 . 5E3
.9 . 8E2
.4.9E2
26.' 00 271-00 Time
Voltage SIR 70S Noise: 52
0.05%,208.0,1.00»,
TRIANGLE LABS Text:TLI#45399 M23-O-3
1003
80:
60:
40:
20.
0:
231-00'
'24:00
File:S982305 #1-746 Acq:18-APR-1998
317.9389 F:2 BSUB( 256, 30, -3'. 0) PKD(9
11:24:51 EH-
,5,5,
Al.
1
2S':00'
F, T) Exp:NDB5US
INJ. TIME -
'<9E6
^
11:26
4.5E5
_3 , 6£5
_2.7Z5
_1 . 8E5
-9 . OE4
O.OEO
' 26\00 271-00' ' ' Time
Voltage SIR 70S Noise : 89
0.05%,356.0,1.00%,
TRIANGLE LABS Text:TLI#45399 M23-0-3
1003.
aol
60:
40:
201
0
23:00
',
;' ' ' '24:00
File:S982305 #1-746 Acq: 18-APR-1998
330.9792 F:2 Exp:NDB5US
A2.
|
j
' 25 1- 00
F, T; Elp:NDB5US
INJ. TIME =
12E6
\
11:26
6.5E5
'.5.2E5
.3.9E5
.2.6E5
.1 . 3E5
O.OEO
'26-00 27^00 ' Time
11:24:51 EI+ Voltage SIR 70S
TRIANGLE LABS Text:TLI#45399 M23-O-3
1003
80.
60.
40.
20.
0.
22:24 22:52
"~~ 23:00
' 23 : 28 23
:55
\^>f^/\^-
24 : 21
* — •—-*,• -v^/
' 24 1- 00
7ile:SP82305 #1-746 Acq:18-APR-1998
375.8364 F:2 Exp:»I>B5US
25,
•*. — *~^s*~s~~^
25:00
INJ. TIME -
•,14 25:49
\^^^—v/^w^N/"*X*^/'
11:26
26:17 26:38 27:13
V-.^/'y^j., — _/*^»».^V. __-^— i-u«f».»/V *n»^'n
1 . 9E6
..1 . 6E6
-1.2E6
.7.8E5
.3.9E5
O.OEO
'26:00 27: 00' ' ' Time
11:24:51 EI+ Voltage SIR 70S
TRIANGLE LABS Text:TLI#45399 M23-0-3
100.
80.
60.
40.
20.
0.
22:29
vwjiAJLtf^^
23:00
•' -5
I 24:01
/^AAAy^y-vv>/^x*A•A/^
~ t
INJ. TIME -
26
T;. n;
24:33 25:00 JT" . 2g . »
24 .' 00
v -if
25:00
• ' • i
11:26
•• 05 rl . 6E3
27:04
26:39 . II 1 11
y\fr*-A\*S^*~-l\/\trSvlk~
-------
File:S982305 #1-746 Acq:18-APR-1998 11:24:51 EI+ Voltage SIR 70S HoimetSO
319.8965 F:2 BSUB(256,30,-3.0) PKD(7,5,3,0.05\,200.0,1.00\,T,T) ExptNVBSUS
TRIANGLE LABS Text:TLI*45399 M23-O-3 INJ. TIME - 11:26
100* 23 39
24:00 ; 25:00 26:00
file:S982305 #1-746 Acq:18-APR-1998 11:24:51 EI+ Voltage SIR 70S Noiae:39
321.8936 F:2 BSUB(256,30,-3.0) PKD(7,5,3,0.051,156.0,1.00\,F,T) Ezp:NDB5OS
TRIANGLE LABS Text:TLI#45399 M23-O-3 INJ. TIME - 11:26
100*
24:00 25:00 26:00
File:S982305 #1-746 Acq:18-APR-1998 11:24:51 EI+ Voltage SIR 70S Noise:134
331.9368 F:2 BSUB(256, 30, -3. 0) PKD(7, 5,3,0.OS\,536.0,1. 00*,F,T) Exp:NDB5US
TRIANGLE LABS Text:TLI#45399 M23-0-3 INJ. TIME - 11:26
100* A2.16E6
80:
60:
40:
20:
0.
80:
60:
40.
20:
24:42
2700
27-00
24:00 25:00 26:00
File:S982305 #1-746 Acq:18-APR-1998 11:24:51 EI+ Voltage SIR 70S Noise:70
333.9338 F:2 BSUB(256,30, -3. 0) PKD(7, 5,3,0.051,280.0,1.00*,F,T) Exp:tWB5US
TRIANGLE LABS Text:TLI#45399 M23-O-3 INJ. TIME = 11:26
27:00
File:S982305 #1-746 Acq:18-APR-1998 11:24:51 EI+ Voltage SIR 70S Noiae:57
327.8847 F:2 BSUB(256, 30,-3 . 0 ) PKD(7, 5,3 , 0 .051,228.0, 1. 00*,F,T) Exp:NDB5US
TRIANGLE LABS Text:TLI#45399 M23-0-3 INJ. TIME = 11:26
1003, A2.40E6
80:
60:
40:
20:
OJ
T
-r
24:00 25:00 26:00
File:S982305 #1-746 Acq:18-APR-1998 11:24:51 EI+ Voltage SIR 70S
330.9792 F:2 Exp:NDB5US
TRIANGLE LABS Text:TLI#45399 M23-O-3 INJ. TIME - 11:26
27:00
8.2E2
.6.5E2
.4.9E2
'-.3.3E2
.1. 6E2
O.OEO
Time
Time
6.1E5
.4.9E5
-3.7E5
.2.4E5
UU3
80:
60:
40:
20:
0:
AH.t7E6
L m
if ^
ft
y W v
24 : 00 25: 00 26: 00 27: 00
O.OEO
Time
5.9E5
4.4E5
3.0E5
1.5E5
O.OEO
Time
6.8E5
5.5E5
4.1E5
2.7E5
1. 4E5
O.OEO
Time
00]
60:
40:
20:
o'-
23:55 24-21 24-38 ^V^vL^ 25:45 26:17 26:38 27:13
, '
24:00 25:00 26:00 271-00
1.9E6
.1. 6E6
.1.2E6
.7.8E5
.3.9E5
O.OEO
Time
258
-------
'ile.-S98.2305 #1-746 Acq:18-APR-1998 lli24tSl SI+ Voltage SIR 70S Noima,36
339.8597 F:2 BSVB(256,30, -3. 0) PKD(7,5,3, 0. 05\, 144. 0, 1. 00\,f, T) ExptNDBSUS
TRIANGLE LABS Text:TLI#45399 M23-O-3 INJ. TIME - 3.1:26
1001 29:11
28:00 29100 30:00
rile:S982305 #1-746 Acq:18-APR-1998 11:24:51 EI+ Voltage SIR 70S Noise,45
341.8567 ri2 BSUB(256,30, -3.0) PKD(7,5,3, 0.05%, 180.0,1.00\,F,T) ExpsKDBSUS
TRIANGLE LABS Text:TLI#45399 M23-0-3 IHJ. TIME - 11:26
1001
31:00
80.
6ol
40.
201
0-
26:21
29:54
28:00 29:00 30:00
File:S982305 #1-746 Acq:18-APR-1998 11:24:51 EI+ Voltage SIS 70S Noise:J7
351.9000 F:2 BSUB(256, 30,-3. 0) PKD(7,5,3, 0.05\,148.0,1. 00*,f, T) Exp:NDB5US
TRIANGLE LABS Text:TLI#45399 H23-0-3 JWJ. TIME - 11:26
1004 A1.74E6 A1.75E6
601
40:
201
31: 00
Oj
28:00 25:00 JOl-00
File:S982305 #1-746 Acq:18-APR-1998 11:24:51 EH- Voltage SIR 70S Noise:37
353.8970 F:2 BSUB(256,30r-3.0) PKS( 7,5, 3, 0. 054,148. 0,1. 00%,F, T) ExpsNDBSUS
TRIANGLE LABS Text:TLI#45399 M23-0-3 INJ. TIME = 11:26
1001, - A1.1SE6 A1.12E6
60.
401
20:
Oj / I I
31: 00
28:00 29:00 30:00
File:S982305 #1-746 Acq:18-APB-1998 11:24:51 EH- Voltage SIR 70S
330.9792 F:2 Exp:NVB5US
TRIANGLE LABS Text:TLI#*5399 M23-0-3 INJ. TIME '
31: 00
1003
80J
601
401
201
0.
11:26
27:13
29:19
~r
T
28:00 29:00 30:00
File:S98230S #1-746 Acq:18-APR-1998 11:24:51 Eli- Voltage SIR 70S
409.7974 F:2 Exp:NDB5US
TRIANGLE LABS Text:TLI#45399 M23-0-3 INJ. TIME -
38133 29,59
31:00
11:26
.1.1E3
.8.6E2
.6.5E2
.4.3E2
.2.2E2
.O.OEO
Time
.5.4E5
.4.3E5
.3.2E5
.2.2E5
.1. 1E5
.O.OEO
Time
.3. 7E5
.3.0E5
.2.2E5
.1. 5E5
.7.5E4
O.OEO
Time
.2.0E6
.1. 6E6
.1. 2E6
.8.1E5
.4.1E5
.O.OEO
Time
28:00
29:00
30:00
31:00
259
-------
:S982305 #1-746 Acq:18-APR-1998 11:24:51 EI+ Voltage SIR JOS SO2.se:37
55.8546 1:2 BSUB(256,30, -3. 0) PKD(7,5,3, 0. 05\, 148.0,1.00\,F,T) ExpsMDBSOS
TRIANGLE LABS Text :TLI#45 399 M23-O-3 IKT. TIMS - 11.-.26
1001 29:09
28:24 28:36 28:48 29:00 29:12 29:24 29:36 29:48 30:00 30:12 30:24 30,36 30:48 31:00 31:12
File:S982305 #1-746 Acq:18-APR-1998 11:24:51 EH- Voltage SIX 70S Hoiae:38
357.8516 F:2 BsnB(256,30, -3.0) PKD(7,5,3,0.05\,152.0,1.00\,F,T) Eip:lO)B5US
TRIANGLE LABS Text:TLI#45399 M23-O-3 IJKT. TIME - 11:26
1001
80.
60.
Time
.3.1E2
.1 . 6E2
28:24 28:36 28:48 29:00 29:12 29:24 29:36 29:48 30:00 30:12 30:24 30:36 30:48 31:00 31:12
File:S982305 #1-746 Acq:18-APR-199S 11:24:51 EI+ Voltage SIR 70S Noise:38
367.8949 F:2 BSVB( 256, 30, -3 . 0) PKD(7, 5, 3 , 0.051, 152.0, 1.00*,F,T) Exp:NDB5US
TRIANGLE LABS Text:TLI#45399 M23-O-3 JJW. TIME - 11:26
1003, A1.Q3E6
.O.OEO
Time
BO:
60J
-------
ile:S982305 #1-465 Acq:18-APR-1998 11:24:51 EI+ Voltage SIR 70S Hoiae:61
73.8208 F:3 BSUB<256,30, -3 .0) PKD(7,5,3,O.OS\,244.0,1.00\,r,T) ExpiVDBSUS
TRIANGLE LABS Text:TLI#45399 M23-O-3 INJ. TIME - 11:26
004.
31:36 31:48 32:00 32:12 32:24 32:36 32:48 33:00 33:12 33:24 33:36 33:48 34:00 34:12 34:24 34:36
ile:S982305 #1-465 Acq:18-APR-1998 11:24:51 SI+ Voltage SIR 70S Noiae:48
75.8178 F:3 BSDB(256,30,-3.0) PKD(7,5,3, 0.05\,192.0,1.00\,r,T) Exp:HI>B5US
TRIANGLE LABS Text:TLI#4S399 M23-O-3 XJKT. TIME - 11:26
004 ' A2. 1E3
3l': 36 31:48' 32.'00'32.'12 32:24 32:36 32:48 33:00 33:12 33:24 33:36 33:48 34:00 34:12 34:24 34:36
File.-5982305 #1-465 Acq:18-APR-1998 11:24:51 EI+ Voltage SIR 70S Noiae:79
83.8639 F:3 BSUB(256,30,-3.0) PKD(7,5,3, 0. 05%,316. 0,1. 00%,r,T) Exp:NDB5US
TRIANGLE LABS Tezt:TLI#45399 M23-O-3 JWJ. TIME = 11:26
004 A8.11E5
A8.24E5
Time
A832.58 A584.45
A917.62
O.OEO
Time
80:
60:
20:
0.
A6.33E5
2.5E5
2.0E5
1.5E5
9.9E4
-5.0E4
IO.OEO
31:36 31:48 32:00 32:12 32:24 32:36 32:48 33:00 33:12 33:24 33:36 33:48 34:00 34:12 34:24 34:36
File:S982305 #1-465 Acq:18-APX-1998 11:24:51 EI+ Voltage SIR 70S ltoi.ae-.69
385.8610 F:3 BSOB(256,30,-3.0) PKD(7, 5,3, 0. 05*,276. 0,1. 00%,F, T) Exp:NDB5US
TRIANGLE LABS Text:TLI#45399 M23-0-3 INJ. TIME - 11:26
1003, A1.62E6
801
60l
40:
20.
Al.
A1.29E6
31:36 31:48 32:00 32:12 32:24 32:36 32:48 33:00 33:12 33:24 33:36 33:48 34:00 34:12 34:24 34:36
File:S982305 #1-465 Acq:18-APR-1998 11:24:51 EI+ Voltage SIS 70S
392.9760 F:3 Exp:lWB5US
TRIANGLE LABS Teit:TLI#45399 M23-O-3 INJ. TIME = 11:26
1001 31:45 32:02 32:14 32:30 32:47 32:59 33:14 . 33i37_3.3..i49_ ._ 34:05 .34:15
80:
60:
40:
20:
0.
1.
-8.
.6.
.4.
-.2.
.0.
31:36 31:48 32:00 32:12 32:24 32:36 32:48 33:00 33:12 33:24 33:36 33:48 34:00 34:12 34:24 34:36
File:S982305 #1-465 Acq:18-APR-1998 11:24:51 EH- Voltage SIR 70S
445.7555 F:3 Elp:NDB5US
TRIANGLE LABS Teit:TLI#45399 M23-0-3
1001
80:
60:
40J 3i,4a 32,13
A >
20:
o:
IKJ. TIME
11:26
34
33:01
33:23
34:03
09
34:2434:34
31:36 31:48 32:00 32:12 32:24 32:36 32:48 33:00 33:12 33:24 33:36 33:48 34:00 34:12 34:34 34:36
Time
7E5
7E5
8E5
9E5
4E4
OEO
T±m<
OE6
OE5
OE5
,OE5
,OE5
.OEO
Tim
.6E3
.9E3
,2E3
,SE3
.3E2
.OEO
Tim
26
-------
tile:s982305 #1-465 Acq:lB-ApR-199B 11,34,51 SI+ Volfaiga SIS 70S )toi,.:49
389.8156 Fs3 BSUB(256,30, -3.0) PKD(7,5,3, 0.05\,196.0,1.00\,T,T) Exp:tWB5DS
TRIANGLE LABS Text:TLI#45399 M23-O-3 IHJ. TIKE - 11:26
Al. 81E3
32:12 32:24 32:36 32:48 33:00 33:12 33:24 33:36 33:48
r±lesS982305 #1-465 Acq:18-APR-1998 11:24:51 SI+ Voltage SIX 70S Xoiae:64
391.8127 F:3 BSUB(256,30, -3.0) PKD(7,S,3, 0.051,256. 0,1. 00\,F,T) Exp-.NDBSUS
TRIANGLE LABS Text:TLI#45399 M23-O-3 JKJ. TIME ' 11:26
1003,
34:00 34:12
32:12 32:24 32:36 32:48 33:00 33':12 33:24 33:36 33:48
File:S982305 #1-465 Acq:lB-APR-1998 11:24:51 EH- Voltage SIX 70S Noise:81
401.8558 F:3 BSUB(256, 30, -3 . 0) PKD( 7, 5,3, 0. 05%, 324 . 0, 1. 00%,F, T) Exp:NDB5US
TRIANGLE LABS Text:TLI#45399 M23-O-3 INJ. TIME - 11:26
10 °4 A1.64E6
34:00 34:12
so:
60L
401
20:
Al.12E6
T
T
~r
32:12 32:24 32':36 32:48 33:00 33:12 33':24 33:36 33:48
File:S982305 #1-465 Acq:18-APS-1998 11:24:51 EI+ Voltage SIR 70S Noiae:121
403.8529 F:3 BSUB<256,30, -3. 0) P1O>(7, 5,3, 0. 051,484. 0,1. 00\,F, T) Exp:NDB5US
TRIANGLE LABS Text:TLI#45399 M23-0-3 JWJ. TIME = 11:26
A1.37E6
i i I i '
34 : 00
34 :12
80.
60.
40.
20.
A9.08E5
32:12 32:24 32:36 32:48 33:00 33:12 33:24 33:36
File:S982305 #1-465 Acq:18-APS-1998 11:24:51 EI+ Voltage SIR 70S
392.9760 F:3 Exp:NDBSOS
TRIANGLE LABS Text:TLI#45399 M23-O-3 JJTJ. TIME
1004
80.
60.
401
20.
0.
33:48 34:00
11:26
i i I i i
34:12
32:12 32:24 32^36 32-48 33:00 33:12 33\24 33\36 ' '33\4S
34\6d ' '34:12
Time
3.7E5
2.7E5
1. 8E5
9.1E4
O.OEO
Time
3. 8E5
3.0E5
2.3E5
.1. 5E5
.7.5E4
.O.OEO
Time
.1. OE6
.8.0E5
6.0E5
4.0E5
2.0E5
O.OEO
Time
262
-------
•ile:S982305 #1-569 Acq:18-APR-1998 11:24:51 EI+ Voltage SIR 70S Noise: 78
407.7818 F:4 BSUB(256,30, -3. 0) PKD(7,5,3, 0. 05\,312. 0,1. 00*,F, T) Exp:NDB5US
TRIANGLE LABS Text:TLI#45399 M23-O-3 Z1K7. TIME - 11:26
-1004
35:48 36:00 36:12 36:24 36:36 36:48 37*00 37:12 37:24
File:S982305 #1-569 Acq:18-APR-1998 11:24:51 EH- Voltage SIR 70S Noiae:57
409.7789 F:4 BSUB(256,30,-3.0) MOJf 7,5,3,0.05\,228. 0,1.00%,y,T; Exp.-NPBSDS
TRIANGLE LABS Text:TLI#45399 M23-O-3 JK7. TIME - 11:26
1003
ao:
35:48 36:00 36:12 36:24 36:36 36:48 37:00 37:12 37':24
File:S982305 #1-569 Acq:18-APR-1998 11:24:51 EI+ Voltage SIR 70S Noise:79
417.8253 F:4 BSUB(256,30, -3 . 0) PKD(7, 5,3, 0. 05%, 316. 0, 1. 00\,F, T) Ezp:lO>B5US
TRIANGLE LABS Text:TLI#45399 M23-O-3 INJ. TIME - 11:26
100* A4.07E5
80.
60.
40.
201
A2.05E3
Al.61E3
37:36
37:48
37:36
37:48
80:
60:
40:
A3.OSES
35:48 36:00 36:12 36:24 36:36 36:48 37:00 37:12 37:24
File:S982305 #1-569 Acq:18-APR-1998 11:24:51 EI+ Voltage SIR 70S Noiae:60
419.8220 F-.4 BSUB(256,30, -3. 0) PKD(7,5,3, 0.051,240.0,1.00\,F,T) Ezp-.SDSSUS
TRIANGLE LABS Text:TLI#45399 M23-0-3 INJ. TIME = 11:26
37:36
37:48
1003
sol
60:
40:
20:
o:
A9. 83E5
A7.55E5
35:48 36:00 36:12 36:24 36:36 36:48 37:00 37:12 37:24
F±le:S982305 #1-569 Acq:18-APS-199B 11:24:51 EI+ Voltage SIR 70S
430.9729 F:4 Exp:JfDB5US
TRIANGLE LABS Text:TLI#45399 M23-0-3 INJ. TIME = 11:26
35:55 36:08 36:17 36:30 361.46 36:59 37
37:36
37:48
80:
60:
40:
20.
0:
37:19 37:31 37:39 37:47
35:48 36:00 36:12 36:24 36:36 36:48 37:00 37:12 37:24
File:S982305 #1-569 Acq:18-APS-1998 11:24:51 EI+ Voltage SIR 70S
479.7165 F:4 ExpsNDBSUS
TRIANGLE LABS Text:TLI#45399 M23-O-3 INJ. TIME = 11:26
37:36
37:48
35:48
36t 00
36:12 36:24
36:36
36:48
37:00
37:12 37:24 37>36 37:48
1.2E3
9.3X2
7.0E2
4. 6E2
2.3E2
O.OEO
Time
8.6E4
6.9E4
5. 1E4
.3. 4E4
.1. 7E4
.O.OEO
Time
.2.1E5
.1. 7E5
.1. 3E5
.8.5E4
.4.3E4
.O.OEO
Time
.7.1E5
.5. 6E5
.4.2E5
.2.8E5
1.4E5
O.OEO
Time
-------
'lJ.eiS982305 #1-565 AcqsI8-APR-lS98 11:24:51 SI+ Voltage SIX 70S Holm*sol
23.7766 T:4 BSUB(256,30,-3.0) PXD(7,S,3,O.OS\,2S6.0,1.00\,r,T) ExptSDBSOS
TRIANGLE LABS Text:TLIt45399 M33-0-3 INJ. TIME - 11:26
1001 A1.62S3 A827-80
36:00 36:06 36:12 36:18 36:24 36:30 36:36 36:42 36:48 36:54 37:00 37:06 37:12 37:18
File:S982305 #1-569 Acq:18-APR-1998 11:24:51 EI+ Voltage SIX 70S Noise:52
425.7737 F:4 BSUB(256,30r-3.0) PKD( 7,5,3, 0. 05\,208.0,1. 00\,T,T) Elp:NDB5US
TRIANGLE LABS Text:TLI#45399 M23-O-3 JWJ. TIME - 11:26
1001
ao:
60:
40.
20.
A754.ll
6.1E2
4.9E2
3.7E2
2.4E2
1.2E2
O.OEO
Time
36:00 36':06 36:12 36'ilB 36:24 36:30 36:36 36:42 36:48 36:54 37:00 37:06 37:12 37:18
File:S982305 #1-569 Acq: 18-APR-1998 11:24:51 EI+ Voltage SIX 70S Noiae:92
435.8169 F:4 BSUB(256, 30,-3 .0) PKD( 7, 5,3 , 0 .051, 368.0, 1. 00\,F,T) Exp:NDB5US
TRIANGLE LABS Text:TLI#45399 M23-O-3 INJ. TIME - 11:26
1003, A7.35E5
ao:
60:
40:
20:
36:00 36:06 36:12 36:18 36:24 36:30 36:36 36:42 36:48 36:54 37:00 37:06 37:12 37:18
File:S982305 #1-569 Acq:18-APR-1998 11:24:51 EI+ Voltage SIR 70S Noise:85
437.8140 F:4 BSUB(256, 30,-3 . 0) PKD( 7, 5,3, 0 . 05%, 340 . 0, 1. 00\,F, T) Exp:NDB5US
TRIANGLE LABS Tezt:TLI#45399 M23-0-3 INJ. TIME - 11:26
1001 A7..
80J
60.
40.
20.
o:
9E5
36:00 36:06 36:12 36:18 36:24 36:30 36:36 36:42 36:48 36:54 37:00 37:06 37:12 37:18
File:S982305 #1-569 Acq:18-APR-1998 11:24:51 EH- Voltage SIR 70S
430.9729 F:4 Exp:NDB5OS
TRIANGLE LABS Text:TLI#45399 M23-0-3 INJ. TIME - 11:26
100$ 36:08 36:17 ,36L30 _ JZtf6 36:59 37:0537:10
80.
60.
40:
20.
0.
O.OEO
Time
1. 4E5
.1. 1E5
.8.4E4
.5.6E4
2.8E4
.O.OEO
Time
.1.3E5
.1. 1E5
.8.0E4
.5.3E4
.2.7E4
.O.OEO
Tim-
.6.9E5
.5.5E5
.4.1E5
.2.8E5
.1. 4E5
O.OEO
Tim-
264
-------
file:S98230i #1-5^9 Acgsl8-JU>X-1998 11:24^:51
EI+ Voltage SIS 70S Boise -.4$
441.7428 F:4 BSUB(256,30, -3.0) PKD(7,5,3, 0.05%,195. 0,1.00\,rtT) Exp-.NDBSUS
TRIANGLE LABS Text:TLH45399 M23-O-3
1003
901
801
701
601
501
401
301
201
101
01
Al . 31E3
L_ A ^ . . .. .
36:00 371-00 . 38:00
File:S9B230S #1-569 Acq:18-APR-1998 11:24:51
IJKT. TIME -
39:00 40:00
EH- Voltage SIR 70S Noise: 60
11:26
2.4X4
.2.2X4
.1 . 9E4
_1 . 7E4
_1.4£4
-1.2E4
-9.7E3
-7.2E3
-4.8E3
.2.4 f 3
n nvn
41:00 ' ' ' 42:00 ' Time
443.7399 F:4 BSUB(256 , 30, -3 .0) PKD( 7,5,3, 0. 05\,240. 0, 1 . 00%, F, T) Exp-.NDBSUS
TRIANGLE LABS Text: 2X1*45399 M23-0-3
1003
901
801
701
601
501
401
301
201
101
~-^~~A~A^^JL^JVn rn — — *~^— I iV Y«~~j^JL~
36:00 37TOO 3sToO
File: :S9 82305 #1-569 Acq:18-APR-1998 11:24:51
430.9729 F:4 Eip:NDB5US
TRIANGLE LABS Text.-lXJ#45399 M23-O-3
1003
901
801
701
601
501
401
301
201
101
oi
>'V...36:08 36l*6 37:10 37-47 38-21
361-00 371-00 38^00
JMle:S982305 #1-569 Acq:18-APR-199B 11:24:51
513.6775 F:4 ExptNDBSUS
TRIANGLE LABS Text: 2X1*45399 M23-O-3
1001
901
80.
70.
60.
SO.
40'
30.
20.
101
oi
INJ. TIME -
^^ __-«.-.- - .J> ^ ^^-js
391-00 40 1-00
EI+ Voltage SIR 70S
INJ'. TIME =
39:0639:31 40:06
^^/Vl^Uyv^/v^-vv^Jy^/V^K^w^.Wv^
391-00 401-00
EH- Voltage SIR 70S
INJ-. TIME -
39.-07 40:20
36-09 37:41 I . 1
^UJU^^^
36:00 37:00 38:00
391-00 40:00
11:26
1 . 8E4
™v— rt A
_1 . 6E4
-1.4E4
_1.2£4
-1.11T4
_B.8E3
-7.0E3
-5.3E3
_3.5Z3
_1 . SE3
n nvn
41 100 42s 00 Tine
11:26
7.1J5
41:154f(j^
.6.3E5
.5.6E5
.4.9E5
-4.2E5
.3.5E5
.2 . 8E5
.2.1E5
.1.4E5
1 7 . 1E4
n nrn
41 1-00 ' 42.' 00 ' ' ' riffle
"
11:26
,_4.0£'3
41 • 01 41 ' 30
H^w VP*- •* \ \,i*t \,ff-^- HC
.3.6E3
L3.2E3
12.8E3
.2.4E3
.2.0E3
.1 . 6E3
ll.2E3
18.0E2
.4.0E2
'• n nrn
41:00 42:00 ' Time
-------
ile:S9B2305 #1-56S Acq:lB-APR-l99S 11:24:51 £1+ Voltage SIR 706 tfoif*i43
57.7377 F:4 BSUB(256,30, -3.0) PKD( 7,5, 3, 0.05\,i72.0,1. 00*,F,T) Exp:NSB5US
TRIANGLE LABS Text:TLI#45399 H23-O-3 JK7. TIME - Ili26
004
A f _ n *i M: * •
A 774.70
80J A / \ M . A5S8.01
40-JS 40:42 40i4S 40:54 41:00 41:06
Tile:S982305 #1-569 Acq:18-APR-1998 11:24:51 EI+ Voltage SIR 70S Holes:36
459.7348 T:4 BSUB(256,30, -3 . 0) PKD(7, S,3, 0. 05%,144 . 0,1. 00\,T, T) ElpsNDBSUS
TRIANGLE LABS TextsTLI#45399 M23-O-3 XKT. TIME - 11:26
100* A2.12E3 A2.22E3
A586.39
41:12
40-36 40:42 40:48 40:54 41:00 41:06
F±le:S982305 #1-569 Acq:18-APS-1998 11:24:51 EI+ Voltage SIR 70S Noise:53
469.7779 F:4 BSUB(256, 30, -3 . 0) PKD(7, 5,3, 0 .051,212.0, 1.00*,F,T) Exp:NDB5DS
TRIANGLE LABS Text:TLI#45399 M23-O-3 INJ. TIME - 11:26
10 04 A8.AOE5
41:12
40-36 40': 42 40:48 40:54 41:00 41:06
File:S982305 #1-569 Acq:lB-APR-1998 11:24:51 EI+ Voltage SIR 70S Noiae:42
471.7750 F:4 BSUB(256, 30,-3 .0 ) PKD( 7, 5,3, 0 . 05%, 168. 0, 1. 00\,F, T) ExpsNDBSUS
TRIANGLE LABS Text :TLI#45399 M23-O-3 INJ~. TIME ' 11:26
1004 A1.03E6
80.
60.
40.
20.
41:12
6.9E2
5.5E2
4.1E2
2.8E2
1. 4E2
O.OEO
Time
.7.8E4
.6.3E4
.4.7E4
.3.1E4
.1. 6E4
.O.OEO
Time
.4E4
-7.5E4
-5.6E4
'.3. 7E4
-1.9E4
41: 06
40:36 40:42 40:48 40:54 41:00
File:S982305 #1-569 Acq:18-APR-1998 11:24:51 EI+ Voltage SIR 70S
430.9729 F:4 Eip-.NDBSUS
TRIANGLE LABS Text:TLI#45399 M23-0-3 INJ. TIME - 11:26
1001 40.-5S 41:07
so:
eo:
40:
20:
41:12
.O.OEO
Tim
40:36
40:42
40:48
.5.OE5
.3.8E5
.2.5E5
.1.3E5
40:54
41:00
41 .• 06
41112
O.OEO
Tim
26(
-------
Channel I 338,9782 Peak top
Height ,33 volts Span 288 ppi
Systei file naie
Data file naie
Resolution
Group nuiber
lonlzatlon Mde
SyItching
Refi lasses 29
A 293
B 384
C 386
D 316
E 318
F 328
6 322
H 328
1 331
J 331
K 332
L 334
H*wo
vW
H 342
0 352
P 354
Q 356
R 358
NDB5US
2
El*
VOlTflOE
416,9768
S 368
T 378
U 376
V 418
Ref ,'iass 416,9768 Peak top
Height ,88 volts Span 288 ppi
or*"1
•' •;
-------
File:S982305 #1-746 Acq:l8-APR-1998 11:24:51 EI+ Voltage SIR 70S
303.9016 F:2 Exp:NDB5US
Sample Text:TLI#45399 M23-0-3
100%
80 J
60l
40J
201
INJ. TIME =
24:36 ' ' ' 24:48 25:00 25:12 25:24 25:36
File:S982305 #1-746 Acq:18-APR-1998 11:24:51 EI+ Voltage SIR 70S
305.8987 F:2 Exp:NDB5US
Sample Text:TLI#45399 M23-O-3 INJ. TIME = 11:
100% A6.99E3
80 J
60 j
40J
20J
:26 File Text:TLI#45399 M23»
2.2E3
L1.8E3
L1.3E3
L8.8E2
L4.4E2
LO.OEO
Time
25:48
26:00
26 File Text:TLI#45399 M23»
3.3E3
L2.7E3
L2.0E3
1 - 1
24:36
-i—i—i—i—r
24:48
25:00 25:12 25:24 25:36
File:S982305 #1-746 Acq:18-APR-1998 11:24:51 EI+ Voltage SIR 70S
315.9419 F:2 Exp:NDB5US
Sample Text:TLI#45399 M23-O-3 INJ. TIME = 11
100% 25:15
80 j
60J
401
20 j
2548
2'elob
^6.7E2
LO.OEO
Time
0.
26 File Text:TLI#45399 M23»
r-4.
24:36
-i—i—|—r-
24:48
25lob
25:12
25\24
25!36
25:48
26:00
L3.6E5
12.7E5
L1.8E5
_9.0E4
O.OEO
Time
-------
Pages 269 through 339 from the Triangle Laboratories, Inc. analytical report
have been excluded by PES since these pages present results for samples
collected at another lime kiln facility during the same mobilization.
-------
TLI Project:
Client Sample:
45399
M23-FB-3
Method 23 PCDD/PCDF Analysis (a)
Analysis File: S982309
Client Project:
Sample Matrix:
TLI ID:
Sample Size:
Dry Weight:
GC Column:
r012.002/Lime Kiln
M23
204-92-11A-D
1.000
n/a
DB-5
Date Received:
Date Extracted:
Date Analyzed:
Dilution Factor:
Blank File:
Analyst:
04/01/98
04/03/98
04/18/98
n/a
U980780
DL
Spike File:
ICal:
ConCal:
% Moisture:
% Lipid:
% Solids:
SPMIT204
SF51078
S982303
n/a
n/a
n/a
Anafytes
2,3,7,8-TCDD
1,2,3,7,8-PeCDD
1,2,3,4,7,8-HxCDD
1,2,3,6,7,8-HxCDD
1,2,3,7,8,9-HxCDD
1,2,3,4,6,7,8-HpCDD
1,2,3,4,6,7,8,9-OCDD
2,3,7,8-TCDF
1,2,3,7,8-PeCDF
2,3,4,7,8-PeCDF
1,2,3,4,7,8-HxCDF
1,2,3,6,7,8-HxCDF
2,3,4,6,7,8-HxCDF
1,2,3,7,8,9-HxCDF
1,2,3,4,6,7,8-HpCDF
1,2,3,4,7,8,9-HpCDF
1,2,3,4,6,7,8,9-OCDF
Totals
Total TCDD
Total PeCDD
Total HxCDD
Total HpCDD
Total TCDF
Total PeCDF
Total HxCDF
Total HpCDF
Amt (ng)
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
... ''•' /:::>fi:*!*^ $8)
ND
ND
ND
ND
ND
ND
ND
0.008
^*'St^ aipe^ $**&'' *«*fer > ** -a
'
0.003
0.005
0.005
0.005
0.005
0.006
0.008
0.002
0.004
0.004
0.004
0.003
0.004
0.004
0.005
0.006
0.006
Number DL EMPC
0.003
0.005
0.005
0.006
0.002
0.004
0.004
1
T^c$Wi*
—
Flags
—
Page 1 of2
MTT2.JSRYl.Q4. LARS 6.11.00
Triangle Laboratories, Inc.®
801 Capitola Drive • Durham, North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 20:27 04/20/98
-------
TLI Project:
Client Sample:
45399
M23-FB-3
Method 23 PCDD/PCDF Analysis (a)
Analysis File: S982309
Internal Standaras
l3C.2-2,3,7,8-TCDF
13C,2-2,3,7,8-TCDD
13C,2-l,2,3,7,8-PeCDF
13C12-l,2,3,7,8-PeCDD
l3d2-l,2,3,6,7,8-HxCDF
'3C,2-l,2,3,6,7,8-HxCDD
13C.2-l,2,3,4,6,7,8-HpCDF
13Ci2-l,2,3,4,6,7,8-HpCDD
13C1:-1,2,3A6,7,8,9-OCDD
Surrogate Standards {Type A}
13C,i-2,3,4,7,8-PeCDF
13Ci2-l,2,3,4,7,8-HxCDF
13Ci2-l,2,3,4,7,8-HxCDD
13C,2-l,2,3,4,7,8,9-HpCDF
Other Standard
«__v . -Jt \
Aim. (ugj
2.6
2.5
2.6
3.0
3.4
3.9
3.3
4.0
8.3
Arnt. (ng)
4.0
3.3
3.6
3.4
Amt (ng)
'^--> , i
1., IH?****^ ,
63.8
63.4
64.2
74.3
84.5
97.8
82.6
99.2
104
;: % Recovery
99.6
83.7
90.3
85.4
% Recovery
^ *W* t •^i.S*'v^'
-«e-fc«Bl^^;;
40%-130%
40%-130%
40%-130%
40%-130%
40%-130%
40%-130%
25%-130%
25%-130%
25%-130%
QC Limits
40%-130%
40%-130%
40%-130%
25%-130%
QC Limits
r4 fr^tt.0^
"... *$%~<%ii>
0.72
0.79
1.53
1.49
0.50
1.21
0.43
1.00
0.85
Ralto
1.53
0.50
1.20
0.41
'* 1M-- iff
^..j^f.
25:15
25:57
29:10
30:13
32:45
33:28
35:46
36:53
40:45
f*i\
29:53
32:39
33:22
37:25
«T -
Et»M* ^' '
Flags
___
*=fe|JS
—
Fkg*
37Cl.-2,3,7,8-TCDD
3.8
93.8
40%-130%
25:59 _
Alternate Standards (Type AJf:;- C: tAmt. (ng
| % Recover/
QC Limits
Ratio
RT
Ftegs
13C,2-l,2,3,7,8,9-HxCDF
13C,2-2,3,4,6,7,8-HxCDF
3.5
3.5
88.0
87.6
40%-130%
40%-130%
0.50
0.50
34:04
33:16
Recovery Standards
Ratio
flT
Flags
1JCu-l,2,3,4-TCDD
13C,2-l,2,3,7,8,9-HxCDD
0.79
1.20
25:47
33:48
Data Reviewer..
Page 2 of 2
04/20/98
MTT2J>SR vl.04. LARS 6.11.00
Triangle Laboratories, Inc.®
801 Capitola Drive • Durham, North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 20:27 04/2CV98
* 341
-------
Data Review By:
Initial ....Date...
f- Xj&jl*
ilculated Noise Area:
0.12
The Total Area for each peak with an ion abundance ratio outside
ratio limits has been recalculated according to method requirements.
Page No.
04/20/98
Listing of S982309B.dbf
Hatched GC Peaks / Ratio / Ret. Time
Compound/
M_Z.... QC.Log Omit Why . .RT. OK Ratio Total.Area... Area.Peak.1. . Area.Peak.2. . Rel.RT Compound.Name.. ID.. Flags.
TCDF
304-306
DC NL 0:
00
0.
RO
DC SN 22:52
D
304-306
13C12-TCDF
316-318
316-318
TCDD
320-322
320-322
37C1-TCDD
328
328
13C12-TCDD
332-334
d SN 25:
16
RO
65-0.89
1.
0.
1.
00
71
24
0 Peaks
DC NL 0:
DC WL 24:
24:
24:
25:
25:
00
13
31
51
15
41
0.
RO
RO
RO
0
0
0
0
.19
.24
.58
.00
65-0.89
0.
0.
0.
0.
0.
1.
4 Peaks
DC NL 0:
DC SN 23:
DC SN 23:
DC SN 25:
DC SN 26:
00
30
38
48
53
0.
RO
RO
RO
RO
94
69
52
76
72
26
0
10
0
2
391
1
396
rn^rv
65-0.89
0.
0.
0.
2.
1.
89
40
50
33
25
0 Peaks
0
0
0
0
0
0
.32
.72
.76 0.33
.95 1.27
.25 163.35
.29 0.92
.25
.17
.14
.05
.05
.07
.00
0.873-1.075
0.
0.
1.
000
906
001 2378-TCDF
AN
0.960-1.040
0.
0.
0.64 0.
1.68 0.
227.90 1.
0.73 1.
000
959
971
984
000 13C12-2378-TCDF
017
ISO
0.899-1.046
0.
0.
0.
0.
1.
000
906
911
994
036
•
0.923-1.077
DC NL 0:
24:
25:
00
37
59
2 Peaks
DC NL 0:
24:
00
48
0,
RO
25:47
25:57
26:17
332-334
PeCDF
340-342
0
2
265
268
.15
.19 2.19
.97 265.97
.16
.65-0.89
2.
0.
0.
0.
0.
4 Peaks
DC NL 0:
:00
DC SN 27:24
1
RO
RO
08
79
79
79
79
0
1
427
298
4
732
tnf+T\
.32-1.78
0.
2.
,75
,67
0
0
.21
.75 0.77
.43 188.52
.81 132.23
.88 2.16
.87
.15
.08
0.
0.
1.
0.923-
0.
0.98 0.
238.91 0.
166.58 1.
2.72 1.
000
949
001 37C1-TCDD
1.077
000
956
994 13C12-1234-TCDD
000 13C12-2378-TCDD
013
-
CLS
RSI
IS1
0.928-1.063
0.
0.
000
939
Triangle Laboratories, Inc.® Analytical Services Division
801 Capitola Drive • Durham, North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 20:27 04/20/98
34
2
-------
Page No.
04/20/98
Listing of S982309B.dbf
Matched GC Peaks / Ratio / Ret. Time
Confound/
M_Z.... QC.Log Omit Why ..RT. OK Ratio Total.Area... Area.Peak.1.. An
•ea.Peak.2.. Rel.RT Compound.Name.. ID.. Flags.
340-342
13C12-PeCDF
352-354
N
352-354
PeCDD
356-358
356-358
13C12-PeCDD
368-370
368-370
HXCDF
374-376
374-376
13C12-HXCDF
384-386
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
SN
SN
SN
SN
0
NL
7
NL
SN
SN
SN
SN
SN
SN
SN
SN
SN
0
NL
SN
SN
SN
SN
3
NL
SN
0
NL
28:37
28:57
29:10
29:21
Peaks
0:00
28:19
28:48
29:10
29:19
29:28
29:53
30:14
Peaks
0:00
28:25
28:37
28:48
28:55
29:39
29:45
29:52
30:02
30:14
Peaks
0:00
29:17
29:28
29:55
30:13
30:21
31:00
31:08
Peaks
0:00
32:39
Peaks
0:00
RO
RO
RO
1.
RO
RO
1.
RO
RO
RO
RO
RO
RO
RO
RO
RO
1.
RO
RO
RO
RO
RO
RO
1.
RO
1.
0.
1.
0.
00
47
67
85
0.
0.
0.
0.
0.
10
12
24
18
00
32-1.78
1.
1.
1.
1.
1.
1.
1.
0.
32-
0.
2.
1.
1.
1.
1.
0.
2.
0.
1.
32-
1.
1.
1
1
1
1
2
1
38
41
46
53
50
22
53
86
•1.78
78
20
22
00
29
75
89
.00
.25
.22
-1.78
.13
.30
.00
.15
.49
.35
.20
.00
.05-1.43
1
1
.10
.00
0.
16.
0.
295.
1.
2.
285.
0.
602.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
189.
16.
0.
0.
19
50 9.66
64 0.38
06 178.65
85 1.11
01 1.22
67 172.84
49 0.30
22
12
13
18
12
15
11
13
13
05
18
00
15
79 0.48
13
25
61 113.32
88 9.69
13
15
0.981
0.993
1.000 12378-PeCDF
1.006
0.863-1.137
0.000
6.84 0.971
0.26 0.987
116.41 1.000 13C12-PeCDF 123
0.74 1.005
1.00 1.010
112.83 1.025 13C12-PeCDF 234
0.35 1.037
0.937-1.022
0.000
0.940
0.947
0.953
0.957
0.981
0.985
0.988
0.994
1.001 12378-PeCDD
0.868-1.132
0.000
0.37 0.969
0.975
0.990
76.29 1.000 13C12-P6CDD 123
7.19 1.004
1.026
1.030
AN
IS2
SUR1
AN-
IS3
207.28
• Pftf Of} / Hvf T\V Wrtl 1 j-Miie
0.
0.
21
23
0.963-1.048
0.000
0.997 123478-HxCDF
AN
0.00
0
RO
.43-0.59
0
.82
0.26
0.878-1.122
0.000
Triangle Laboratories, Inc.® Analytical Services Division
801 Capitola Drive • Durham, North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 20:27 04/20/98
-------
Page No.
04/20/98
Listing of S982309B.dbf
Hatched GC Peaks / Ratio / Ret. Time
Compound/
M_Z.... QC.Log Omit Why ..RT. OK Ratio Total.Area... Area.Peak.1.. Area.Peak.2. . Rel.RT Confound. Name.. ID.. Flags.
384-386
HxCDD
390-392
390-392
13C 12 -HxCDD
402-404
402-404
HpCDF
408-410
408-410
13C12-HpCDF
418-420
418-420
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
SN
6
NL
SN
SN
SN
SN
SN
SN
SN
SN
WH
WH
0
NL
WL
SN
SN
4
NL
1
NL
SN
SN
2
31:41
31:48
32:39
32:45
33:05
33:16
34:04
Peaks
0:00
32:39
32:50
32:52
33:00
33:14
33:21
33:46
33:51
33:58
34:04
Peaks
0:00
32:24
32:50
33:22
33:28
33:48
34:10
34:14
Peaks
0:00
35:45
Peak
0:00
35:46
36:04
36:14
37:25
Peaks
1.
RO
RO
RO
RO
RO
RO
RO
RO
RO
1.
RO
RO
RO
0.
0
RO
RO
RO
0.
0,
0
0
0
0
0
.50
.51
.50
.50
.47
.50
.50
1
3.
5.
229.
269.
0.
276.
223.
.008.
UvS*T\V
05-1.43
1
0
0
5
0
10
2
0
1
0
1
.25
.47
.80
.00
.80
.00
.17
.57
.67
.50
.21
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
31 1.10
66 1.92
34 76.70
70 89.65
28
81 91.85
24 73.94
06
18
14
07
04
07
04
13
07
07
05
31
00
05-1.43
1
1
1
1
1
1
0
1
.88
1
0
.17
.00
.18
.20
.21
.20
.71
.88
-1.20
.08
.96
0.
0.
1.
187.
226.
250.
0.
0.
665.
vivf^nr
HXL.UL
0.
0.
0.
26
20
44 0.78
67 102.18
09 124.00
31 136.48
22
18
51
25
47 0.23
47
.37-0.51
0
0
1
1
0
.92
.43
.38
.33
.41
0.
175.
0.
0.
119.
295.
19
18 52.41
19
17
85 34.77
.03
2.21 0
3.74 0
152.64 0
180.05 1
1
184.96 1
149.30 1
.967
.971
.997 13C12-HXCDF 478
.000 13C12-HXCDF 678
.010
.016 13C12-HXCDF 234
.040 13C12-HXCDF 789
SUR2
1 34
ALT2
ALT1
0.958-1.014
0
0
0
0
0
0
0
1
1
1
1
.000
.976
.981
.982
.986
.993
.997
.009
.011 123789-HxCDD
.015
.018
AN
0.970-1.030
0
0
0.66 0
85.49 0
102.09 1
113.83 1
1
1
0.997
0
0.24 1
.000
.968
.981
.997 13C12-HXCDD 478
.000 13C12-HXCDD 678
.010 13C12-HXCDD 789
.021
.023
-1.051
.000
.000
SUR3
IS5
RS2
0.944-1.112
0
122.77 1
1
1
85.08 1
.000
.000 13Cl-2-HpCDF 678
.008
.013
.046 13C12-HpCDF 789
IS6
SUR4
Triangle Laboratories, Inc.® Analytical Services Division
801 Caprtola Drive • Durham, North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 20:27 04/20&4 4
-------
Page No. 4
04/20/98
Listing of S982309B.dbf
Matched GC Peaks / Ratio / Ret. Time
Compound/
M_Z.... QC.Log Omit Why ..RT. OK Ratio Total.Area... Area.Peak.1.. Area.Peak.2.. Rel.RT Compound.Name.. ID.. Flags.
Above: HpCDF / HpCDD Follows
HpCDD
424-426
424-426
0.88-1.20
DC NL 0:00 1.17
0 Peaks
0.26
0.00
0.976-1.005
0.000
13C12-HpCDD 0.88-1.20
436-438 DC NL 0:00 1.18 0.37
36:04 RO 0.77 . 1.55
36:53 1.00 183.78
436-438 2 Peaks 185.33
0.79
91.68
0.973-1.027
0.000
1.03 0.978
92.10 1.000 13C12-HpCDD 678 IS7
OCDF
442-444
442-444
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
NL
SN
SN
SN
SN
SN
SN
SN
SN
SN
SN
SN
0
0
38
39
39
39
39
39
39
39
40
42
42
:00
:48
:01
:07
:14
:23
:34
:42
:52
:22
:27
:38
0.
RO
RO
RO
RO
RO
RO
RO
RO
RO
RO
76-1.02
1.
1
0.
0,
0
0
0
1
2
1
1
1
.00
.25
.20
.36
.52
.30
.17
.75
.00
.30
.00
.67
Peaks
Above: HpCDD / Octa-CDD and CDF Follows
0.20
0.15
0.04
0.08
0.23
0.06
0.02
0.15
0.08
0.19
0.16
0.06
0.00
0.902-1.098
0.
0.
0.
0.
0.
0.
0.
0,
0,
0,
1.
,000
.952
.957
.960
.963
.966
.971
.974
.978
.991
.042
1.046
OCDD
458-460
453-460
0.76-1.02
DC NL 0:00 0.80
d SN 40:47 0.91
DC SN 40:56 RO 2.13
0 Peaks
0.18
0.61
0.15
0.00
0.902-1.098
0.000
1.001 OCDD
1.004
AN
13C12-OCDD 0.76-1.02
470-472 DC NL 0:00 RO 1.14 0.13
40:45 0.85 260.38
DC WH 41:17 RO 2.15 0.25
470-472 1 Peak 260.38
119.82
0.996-1.004
0.000
140.56 1.000 13C12-OCDD
1.013
IS8
Column Description "Why" Code Description QC Log Desc.
M_Z -Nominal Ion Mass(es)
. .RT. -Retention Time (mn:ss)
Rat.l -Ratio of M/M+2 Ions
OK -RO=Ratio Outside Limits
Rel.RT-Relative Retention Time
End of Report ***
WL-Below Retention Time Window A-Peak Added
WH-Above Retention Time Window
SN-Below Signal to Noise Level
-------
•ile:S982309 #1-746 Acq:18-APS-1998 14:27:30 XI+ Voltage SIS 70S Hoist: 53
303.9016 F:2 BSUB(256, 30, -3.0) PKD(9, 5, 5, 0. 05%, 212. 0,1 . 00*,F ,T) XxpiNDBSUS
TRIANGLE LABS Text:TLI#45399 H23-FB-3 IKT. TIME - 14:30
A873. 34
23:00 24:00 25:00 25:00
File:S982309 #1-746 Acq: 18-APR-199B 14:27:30 XI+ Voltage SIR 70S Noise-.56
305.8987 F:2 BSUB(256,30,-3.0) PXD(9, 5,5, 0.05\,224.0,1.00\,F, T) ExpsSDBSUS
TRIANGLE LABS Text:TLI#45399 M23-FB-3 INJ. TIME - 14:30
1003, .,11 "7 i""
Al. 36E3
23:00 24:00 25:00 26:00
File:S982309 #1-746 Acq: 18-APR-1998 14:27:30 EI+ Voltage SIR 70S Noiae:86
315.9419 F:2 BSUB(256, 30, -3 . 0) PKD(9r 5, 5, 0. 05%, 344 . 0, 1. 00%,F, T) Exp:NDB5US
TRIANGLE LABS Text:TLI#45399 M23-FB-3 INJ. TIME - 14:30
1001
23:00 24:00 25:00 26:00
File:S982309 #1-746 Acq: 18-APX-1998 14:27:30 EI+ Voltage SIR 70S Noise:91
317.9389 F:2 BSOB(256, 30, -3. 0) PKD( 9, 5,5, 0. 05*,364. 0,1.00\,F, T) Ezp:NDB5US
TRIANGLE LASS Tejct:TLI#45399 M23-FB-3 TJITJ. TIME = 14:30
1003
aol
40
20.
OJ
23:00 , 24:00 . 25:00
File:S982309 #1-746 Acq: 18-APR-1998 14:27:30 EI+ Voltage SIR 70S
330.9792 F:2 Exp:NDB5US
TRIANGLE LABS Tezt:TLI#45399 M23-FB-3 INJ. TIME
1004
801
601
401
201
ol
26:00
14:30
A1.16E3
27:00
27:00
27:00
27:00
23:00 - 24:00 25:00
File:S982309 #1-746 Acq:18-APR-199B 14:27:30 ZI+ Voltage SIR 70S
375.8364 F:2 Exp:NDB5US
TRIANGLE LABS Text:TLI#45399 M23-FB-3 IHJ. TIME -
1004
26': OO'
27:00
14:30
60:.
401
20!
ol
26 35
22:23 22
23:22
, 23:12
24:42
23:53 24
25:26
5:12
26:12
26:03
26:54
23:00
24\00
25:00
'26\QQ
-9.7E2
.7.8X2
-5.8E2
.3. 9E2
.1.9X2
.O.OEO
Time
.O.OEO
Time
4.8E5
3.8E5
2.9E5
1.9E5
9.6E4
O.OEO
Time
6.6E5
5.3E5
4.0E5
.2. 7E5
1.3E5
O.OEO
Time
.1. 2E6
.9. 6E5
.7.2E5
.4.8E5
.2.4E5
O.OEO
Tim,
.1. 8E3
.1. 5E3
.1.1E3
.7.3E2
.3.6E2
.O.OEO
Time
34C
-------
File:S982309 #1-746 Acq:18-APR-1998 14:27:30 XI+ Voltage SIS 70S Noiae:40
319.8965 F:2 BSDB(256r30, -3.0) PKD(7,5,3,0.05\,160.0,1.00\,F,T) Exp:NDB5US
TRIANGLE LABS Text:TLI#45399 H23-FB-3 INJ. TIME - 14:30
lOOi A1.94E3
24:00 • 25:00 26:00
File:S982309 #1-746 Acq: 18-APR-1998 14:27:30 EI+ Voltage SIS 70S Noise:43
321.8936 F:2 BSOB(256,30^-3.0) PKD(7,5,3,0.05\,172.0,1.00\,F,T)
TRIANGLE LABS Text:TLI#45399 M23-FB-3 XKT. TIME - 14:30
A2.17E3 A1.10E3
24:00 25:00 26:00
File:S982309 #1-746 Acq:18-APR-1998 14:27:30 EI+ Voltage SIS 70S Noiae:123
331.9368 F:2 BSUB(256, 30, -3 . 0) PKD(7, 5,3, 0 . 051,492. 0, 1. 00*,F, T) Exp:NI>B5US
TRIANGLE LABS Text:TLI#45399 M23-FB-3 . IKJT. TIME - 14:30
1003, A1.B9E6
27:00
27:00
80.
601
401
201
ol
1.32E6
24:00 25:00 26:00
File:S982309 #1-746 Acq:18-APR-1998 14:27:30 EI+ Voltage SIS 70S Noise:58
333.9338 F:2 BSUB(256,30,-3.0) PKD(7,5,3,0.051,232.0,1.00l,F,T) Exp:m>B5US
TRIANGLE LABS Tezt:TLI#45399 M23-FB-3 INJ. TIME = 14:30
1003, '• A2.39E6
27\00
flOj
60J.
40:
201
1. 67E6
°^ , , , , , , , , , , , , ./ .. ,»
24:00 25:00 26:00
File:S982309 #1-746 Acq:18-APR-199B 14:27:30 EI+ Voltage SIR 70S Noiae:73
327.8847 F:2 BSUBf 256, 30,-3 . 0 ) PKD(7, 5,3, 0 . 051,292. 0, 1. 00*,F,T) Exp:NDB5VS
TRIANGLE LABS Text:TLI#45399 M23-FB-3 IWJ. TIME - 14:30
1003,
80:
40.
27.'00
24:00 25:00 26:00
File:S982309 #1-746 Acq:18-APR-1998 14:27:30 EI+ Voltage SIR 70S
330.9792 F:2 Exp:NDB5VS
TRIANGLE LABS Text:TLI#45399 M23-FB-3 IK7. TIME
25:15 35.49 26il7
I
27:00
1001
Time
4.3E5
3.2E5
2.1E5
.LIES
O.OEO
Time
.6.7E5
.5.3E5
.4.0E5
.2.7E5
.1. 3E5
O.OEO
Tine
.7.7E5
.6.1E5
.4.6E5
.3.1E5
.1.5E5
.O.OEO
Time
24 • 00
25:00
2600
27:00
-------
F±le:S982309 #1-746 Acq:18-APR-1998 14:27:30 XI + Voltage SIR 70S Koi»a:46
339.8597 T:2 BSOB(256,30,-3.0) PKD(7,5,3, 0.05%, 184.0,1.00\,r,T) ExpsODBSVS
TRIANGLE LABS Text:TLI#45399 M23-FB-3 IKT. TIME - 14:30
1004 A2.24E3
28:00 29:00 30:00
File:S982309 #1-746 AcqilS-APR-1998 14:27:30 EI+ Voltage SIS 70S Noife:59
341.8567 Fs2 BSUB(256,30,-3.0) PKD(7, 5,3, O.OS\,236. 0,1.00\,T,T) Xxp-.NDBSUS
TRIANGLE LABS Text:TLI#45399 M23-FB-3 IKJ. TIME - 14:30
1004 A1.75E3
31,00
28:00 29:00 30:00
File:S982309 #1-746 Acq:18-APR-1998 14:27:30 EI+ Voltage SIX 70S Noiae:55
351.9000 F:2 BSUB(256r 30, -3.0) PKD(7,5,3, 0. 051,220. 0,1. 00%,T, T) Exp-.NDBSUS
TRIANGLE LABS Text:TLI#4S399 H23-FB-3 IKJ. TIME = 14:30
31:00
ICOi
40
20.
o
Al 79E6
Al. 73E6
28:00 29:00 30:00
File:S982309 #1-746 Acq:ia-APR-1998 14:27:30 EH- Voltage SIR 70S Noiae:38
353.8970 F:2 BSUB(256,30,-3:0) PKD(7, 5,3, 0. 05%, 152. 0,1. 00*,F, T) Exp:NDB5US
TRIANGLE LABS Text:TLI#45399 M23-FB-3 INJ. TIME - 14:30
100$ A1.16E6 A1.13E6
601
40:
201
31 : 00
1 1 « i» i i i 1 ' i ' i i i *i—* |
28:00 29:00 30:00
File:S982309 #1-746 Acq:1B-APR-1998 14:27:30 EI+ Voltage SIS 70S
330.9792 F:2 Exp:NDB5US
TRIANGLE LABS Text:TLI#45399 M23-FB-3 INJ. TIME -
1004 29JL19
28:4428:59 _/V_/\v. 29:55
40:
20:
o:
31': 00
14:30
28:0029:0030:00
File:S982309 #1-746 Acq:18-APX-1998 14:27:30 EI+ Voltage SIX 70S
409.7974 F:2 Exp:NDB5US
TRIANGLE LABS Text:TLI#45399 M23-FB-3 JH17. TIME -
3l':00
1001
80:
14:30
28:50
.5.6E5
.4.5E5
.3. 4E5
.2.2E5
.1.1E5
.O.OEO
Time
.3. 6E5
.2.9E5
.2.2E5
.1.5E5
.7.3E4
.O.OEO
Time
.1.3E6
.1. OE6
.7.6E5
.5.1E5
2.5E5
O.OEO
Time
28:00
29:00
30:00
31:00
•7k
-------
*ile:S9B2309 #1-746 Acq:18-APR-1998 14:37:30 EI+ voltage sJJ? 70S Noises36
55.8546 F:2 BSUB(256,30,-3.0) PKD( 7,5,3, 0. 05\,144.0,1.00\,r,T) EipiKDBSUS
TRIANGLE LABS Text:TLI#45399 M23-TB-3 HK7. TIME - 14:30
1004 A5.12E3
'.O.OEO
28:24 28:36 28:48 29:00 29:12 29:24 29:36 29:48 30:00 30:12 30:24 30:36 30:48 31:00 31:12 Time
File:S982309 #1-746 Acq: 18-APR-1998 14:27:30 EI+ Voltage SIR 70S Noise:45
357.8516 F:2 BSOB(256,30, -3. 0) PKD(7, 5,3,0.051,180.0,1.00\,F,T) Exp:SDB5US
TRIANGLE LABS Tezt:TLI#45399 M23-FB-3 JJTJ. TIME - 14:30
100*. A1.25E3 -5.3E2
Time
28:24 28:36 28:48 29:00 29:12 29:24 29:36 29:48 30:00 30:12 30:24 30:36 30:48 31:00 31:12
File:S982309 #1-746 Acq: 18-APR-1998 14:27:30 EI+ Voltage SIR 70S Noise:43
367.8949 F:2 BSUB(256, 30,-3.0 ) PKD(7,5, 3, 0. 051,172. 0,1. 00%, F, T) Exp:NDB5US
TRIANGLE LABS Text: TLI#45399' M23-FB-3 INJ. TIME= 14:30
1003, - A1.J.3E6 3.5E5
O.OEO
80.
60.
40:
20.
9. 69E4
-2.8E5
-2.1E5
^.1. 4E5
'.6.9E4
.O.OEO
28:24 28:36 28:48 29:00 29:12 29:24 29:36 29:48 30:00 30:12 30:24 30:36 30:48 31:00 31:12
File:S982309 #1-746 Acq:18-APR-1998 14:27:30 EI+ Voltage SIR 70S Noiae:39
369.8919 F:2 BSUB(2S6, 30,-3 .0 ) PKD(7, 5, 3, 0 . 05%, 156. 0, 1. 00*,F, T) Ejcp:NDB5US
TRIANGLE LABS Text:TLI#45399 M23-FB-3 INJ. TIME = 14:30
1003, A7.6.3E5
Time
80.
60.
40.
20.
0.
7.19E4
.1. 9E5
-1.4E5
'.9. 3E4
-4.7E4
O.OEO
28:24 28:36 28:48 29:00 29:12 29:24 29:36 29:48 30:00 30:12 30:24 30\36 JO:48 31:00 Jll-12 Time
File:S982309 #1-746 Acq:18-APR-1998 14:27:30 Eli- Voltage SIR 70S
330.9792 F:2 Eip:NDB5US
TRIANGLE LABS Text:TLI#45399 M23-FB-3
1003
80.
60.
40.
20.
0.
39:19
28:33 28:44 28:59^29:13
29:32
IHJ. TIME - 14.-30
JO.-05 30:33
-1.3E6
_1.OE6
,7.6ES
.5.1E5
.2.5E5
O.OEO
28:24 28:36 28:48 29:00.. 29:13 39t24 29:36 39:48 30:00 30:12 30:24 30\36 30\48 3lYoO 31\12 Time
-------
file i:S9B2309 #1-465 Acq:18-APR-1998 14:27:30 EI+ Voltage SIS 70S «bi««:57
73.8208 F:3 BSUB(2S6,30, -3. 0) PKD(7,5,3, 0.05%,228.0,1.00\,r,T) Exp:NDB5US
TRIANGLE LABS Text: TLIf 45399 M23-FB-3 ISJT. TIME - 14:30
100
31*:36 31:4(8 3.2 i 00 32:12 32:24 32:36 32:48 33:00 33:12 33:24 33:36 33:48 34:00 34:12 34:24 34:36
•ile:S982309 #1-465 Acq:18-APS-1998 14:27:30 EI+ Voltage SIX 70S Noise:49
375.8178 F:3 BSUS(256,30,-3.0) PKD(7,5,3, 0.05%, 196.0,1. 00\,T, T) Exp:NDB5US
TRIANGLE LABS Tejct:TLI#45399 M23-FB-3 IJKT. TIKE - 14:30
1001
A624.99.
A1.34E3 I I :
$$MkjH\^^^
9E2
9E2
.9E2
.9E2
.OE2
.OEO
Time
31:36 31:48 32:00 32:12 32:24 32:36 32:48 33:00 33:12 33:24 33:36 33:48 34:00 34:12 34:24 34:36
rile:S982309 01-465 Acq:18-APS-1998 14:27:30 EI+ Voltage SIS 70S Noise:68
383.8639 F:3 BSUB(256, 30,-3 .0 ) PKD(7, 5,3, 0 .051,272. 0, 1. 00\,F, T) Exp:NDB5aS
TRIANGLE LABS Text:TLI#45399 H23-FB-3 JJW. TIME - 14:30
1001
60J
40.
201
ol
A8.97E5
A9.18E5
A7.39E5
31:36 31:48 32:00 32:12 32:24 32:36 32:48 33:00 33:12 33:24 33:36 33:48 34:00 34:12 34:24 34:36
File:S982309 #1-465 Acq:18-APR-1998 14:27:30 EI+ Voltage SIR 70S Noise:84
385.8610 F:3 BSUB(256, 30, -3 . 0) PKD( 7, 5, 3, 0 . 05%, 336. 0, 1. 00\,F, T) Exp:KDB5US
TRIANGLE LABS Text:TLI#45399 M23-FB-3 INJ. TIME - 14.-JO
100$ A1.JOE6 A1.85E6 ,-5
80J
601
401
20:
ol
A1.49E6
31:36 31:48 32:00 32:12 32:24 32:36 32:48 33:00 33:12 33:24 33:36 33:48 34:00 34:12 34:24 34:36
File:S982309 #1-465 Acq:18-APR-1998 14:27:30 EI+ Voltage SIR 70S
392.9760 F:3 EipilfDSSUS
TRIANGLE LABS
1001
801
601
401
201
0.
Text:TLI#45399 M23-FB-3
31:4031:50 32:04 32:16 32:27 32:39
r-6.
15.
-3.
-2.
.1.
31:36 31:48 32:00 32:12 32:24 32:36 32:48 33:00 33:12 33:24 33:36 33:48 34:00 34:12 34:24 34:36
F±le:S982309 #1-465 Acq:18-APR-1998 14:27:30 EI+ Voltage SIR 70S
445.7555 F:3 Eip:NDB5US
TRIANGLE LABS Text:TLI#45399 M23-FB-3 INJ. TIME - 14:30
33 54 2
,6E5
.1E5
.6E5
.OE5
.2E4
,OEO
Time
.2E5
.2E5
.1E5
.1E5
.OE5
.OEO
Time
2E5
OE5
7E5
5E5
,2E5
OEO
Tiae
801
601
401
201
01
31:50
32:21 32:36
1 A A H 34''14
VJVwJUA^^A^^Av-^^^
31:36 31:48 32:00 32:12 32:24 32:36 32:48 33:00 33:12 33:24 33:36 33:48 34:00 34:12 34,24 34:36
.2E3
.8E3
.3E3
.8E2
.4E2
.OEO
Time
-------
'ile:S9B2309 tl-465 Acq:18-APR-19S8 14:27:30 EH- Voltage SIR 70S Noia»:50
89.8156 T:3 BSUB(256,30,-3.0) PKD(7,5,3, 0. 051,200. 0,1. 00%,r, T) ElptNDBSUS
TRIANGLE LABS Teit:TLI#45399 M23-TB-3 HKT. TIKE " 14:30
004 A2.04E3 _7.5JE2
.6.0E2
.4.5E2
.3. OE2
.1.5E2
O.OEO
32:12 32:24 32:36 32:48 33:00 33:12 33:24 33:36 33s<8 ' 34:00 ' '34:12 Tia
File:S982309 #1-465 Acq: 18-APR-1998 14:27:30 EI+ Voltage SIS 70S Koise:41
91.8127 T:3 BSOB(256,30,-3.0) PKD(7,5,3, 0. 05\,164. 0,1.00\,F,T) Exp:NDB5US
TRIANGLE LABS Text:TLI#45399 M23-FB-3 INJ. TIME - 14:30
1001 Al. 1E3 _ _7.0r2
32':12 32':24 32:36 32:48 33:00 33:12 33:24 33:36 33:48 34:00
'ile:S982309 #1-465 Acq:18-APR-1998 14:27:30 EI+ Voltage SIS 70S Noise:71
401.8558 F:3 BSUB(256,30;-3.0) PKD(7, 5,3, 0 . 05\,2S4. 0,1. 00%,f, T) Exp:jn>B5US
TRIANGLE LABS Text:TLI#45399 M23-FB-3 IKJ. TIME = 14:30
1003
80J
601
40:
20.
A1.24E6
Al.02E6
A1.36E6
O.OEO
34•12 Time
-3.3E5
12.6E5
.2.0E5
-I.3E5
'. 6. 6E4
32:12 32:24 32:3f 32:48 33:00 33:12 33:24 33:36 33:48
File:S982309 #1-465 Acq:18-APR-1998 14:27:30 EI+ Voltage SIR 70S Noiae:58
403.8529 F:3 BSUB(256,30, -3.0) PKD(7, 5,3, 0. 05%,232. 0, 1. 00\,F, T) Exp:SDBSVS
TRIANGLE LABS Text:TLI#45399 M23-FB-3 INJ. TIKE - 14:30
1004 ,, „„„, A1.14E6
34:00
O.OEO
Tim.
BO:
so:
-------
F±le:S9S2309 #1-569 Aoq:IB-APR-1998 14:27:30 EI+ Voltage SIR 70S Noia»:64
07.7818 F:4 BSUB(256,30,-3.0) PKD(7,5,3,0.05\,256.0,1.00\,F,T) ExpiHDBSUS
TRIANGLE LABS TextsTLI#4S399 M23-FB-3 INJ. TIME - 14:30
100*.
35:48 36': 00 36:12 36:24 36:36 36:48 37:00 37:12 37:24
File:S982309 #1-569 Acq:18-APR-1998 14:27:30 EI+ Voltage SIR 70S Noiae:60
409.7789 F:4 BSUB( 256,30,-3.0) PKD(7,5,3,0,OS\,240.0,1.00\,T,T) EzpsNDBSUS
TRIANGLE LABS Text:TLI#45399 M23-FB-3 I1KT. TIME - 14:30
100* A2.37E3
80:
60:
40:
20:
* ii v * i ~v YV T v"' »-'vv~^\^s\s
35:48 ' 36:00 36:12 ' 36\24 ' 36\36 ' 36:48 37': 00 37:12 37:24
F±le:S982309 #1-569 Acq:18-APR-1998 14:27:30 EI+ Voltage SIR 70S Noise:60
417.8253 F:4 BSUB(256,30, -3. 0) PKD(7, 5,3, 0. 05\,240. 0,1. 00*,F, T) Eip-.NDBSUS
TRIANGLE LABS Tezt:TLI#45399 M23-FB-3 INJ. TIME * 14:30
100* A5.J4E5
80:
60:
40:
20:
oj
A3.48E5
35:48 36:00 36:12 36:24 36:36 36:48 37:00 37:12 37:24
F±le:S982309 #1-569 Acq:18-APR-1998 14:27:30 EI+ Voltage SIR 70S Noise:67
419.8220 F:4 BSUB(256, 30,-3 . 0 ) PKD( 7, 5, 3, 0 . 05%, 268. 0, 1. 00%,f, T) Exp:NDB5US
TRIANGLE LABS Text:TLI#45399 M23-FB-3 INJ. TIME - 14:30
1004 A1.23E6
37:36
37:48
80:
60.
40:
20:
A8.51E5
35:48 36:00 36:12 36:24 36:36 36:48 37:00 37:12
Fils:S982309 #1-569 Acq:18-APR-1998 14:27:30 EI+ Voltage SIR 70S
430.9729 F:4 Exp:m>B5US
TRIANGLE LABS Text:TLI#45399 M23-FB-3 INJT. TIME '
37:24
14:30
1003
80:
60:
40:
20:
0.
35:52
36:53 37:03 37:13
37:36
37:36
37:48
-r
rr
~r
~r
35:48 36:00 36:12 36':24 36:36 36:48 37:00 37:12
F±le:S982309 #1-569 Acq:18-APR-1998 14:27:30 EI+ Voltage SIR 70S
479.7165 F:4 Eip:NDB5US
TRIANGLE LABS Teit:TLI#45399 M23-FB-3 INJ. TIME -
100J
80:
60:
40l
20:
ol
37:24 37:36
37:38
O.OEO
Time
35:
351-48 36s 00
36:24 36:36
36:48
'jViflV ' '37\ 12
37:24 37:36
i i I i i
37:48
O.OEO
Time
C1.1E5
-9.1E4
-6.8E4
.4.5E4
.2.3E4
.O.OEO
Time
.2.7E5
'-.2.2E5
Ll. 6E5
Ll. 1E5
.5.5E4
.O.OEO
Time
-4.2E5
.3. 4E5
-2.5E5
.1. 7E5
.8.5E4
37:48
37:50
O.OEO
Time
2.0E3
.1. 6E3
.1.2E3
.7.8E2
.3.9E2
O.OEO
Tim.
352-
-------
ile:S982309 #1-569 Acq:18-APR-lS98 14:27:30 SI+ Voltage SIR 70S HOi»e:69
23.7766 F:4 BSVB( 256, 30, -3. 0) PKD(7,5,3 ,0.051,276 .0,1.0Q\,F,T) Elp:NDB5US
TRIANGLE LABS Text: TLIf 45399 M23-FB-3 IKJ. TIME - 14:30
004 . Al. 77E3
80.
60:
40.
20:
36,00 36:06 36:12 36:18 36:24 36:30 36:36 36s42 36:48 36:54 37:00 37:06 37:12 37:18
File:S982309 il-569 Acq:18-APR-1998 14:27:30 EI+ Voltage SIR 70S Noise:62
425.7737 F:4 BSUB(256, 30,-3 .0 ) PKD( 7, 5,3, 0. 05\,248. 0, 1.00\,F,T) £zp:HDB5C7S
TRIANGLE LABS Text:TLI#45399 M23-FB-3 INJ. TIME - 14:30
10 04 A1.24E3
80.
60.
40.
20.
A858.29
.5.8E2
.4.6E2
.3. 5E2
.2.3E2
.1.2E2
.O.OEO
Tin,
.6.6E2
.5. 3E2
.4.0E2
.2.6E2
.1. 3E2
36:00 36:06 36:12 36:18 36:24 36:30 36:36 36:42 36:48 36:54 37:00 37:06 37:12 37:18
F±le:S982309 #1-569 Acq:18-APR-199S 14:27:30 EI+ Voltage SIR 70S Noise:98
435.8169 F:4 BSUB(256r 30,-3 .0) PKD(7, 5,3, 0. 05%,392. 0,1. 00\,F, T) Exp:NDB5US
TRIANGLE LABS TeXt:TLI#45399 M23-FB-3 INJ. TIME - 14:30
1004 A9.J.7E5
80.
60.
40.
20.
O.OEO
Time
36:00 36:06 36:12 36:18 36:24 36:30 36:36 36:42 36:48 36:54 37:00 37:06 37:12 37:18
FileiS982309 #1-569 Acq:18-APR-1998 14:27:30 EI+ Voltage SIR 70S Noise:87
437.8140 F:4 BSVB(256 , 30r-3 .0 ) PKD( 7, 5, 3, 0 . 05%, 348 . 0, 1. 00 \,F, T) Exp:NDB5US
TRIANGLE LABS Text:TLI#45399 M23-FB-3 XWJ. TIME = 14:30
1004 A9.J1E5
ao:
60J
40:
20:
1.4E5
1.1E5
8.6E4
'.S.7E4
-2.9E4
36:00 36:06 36:12 36:18 36:24 36:30 36:36 36:42 36:48 36:54 37:00 37:06 37:12 37:18
File:S982309 #1-569 Acq:18-APR-1998 14:27:30 EI+ Voltage SIR 70S
430.9729 F:4 Exp:NDB5US
TRIANGLE LABS Text:TLI#45399 M23-FB-3 JK7. TIME - 14:30
.O.OEO
Tim
1003
80.
60.
40:
20.
36:08
36:39
36:53
37:03
37:13
-4.1E5
-3.3E5
.2.4E5
-1.6E5
.8.1E4
36:00 36:06 36:12 36:18 36:24 36:30 36t36 36s42 36>48 36:54 37:00 37:06 37:12 37:18
O.OEO
Tim
-------
File:S982309 #1-569 Acq:18-APR-1998 14:27
441.7428 F:4 BSUB(256, 30, -3 .0) P1O>(7,5,3,
TRIANGLE LABS Text:TLI#45399 M23-FB-3
1001
901
a 01
701
601
501
401
301
20\
101
36:00 37:00 38:00
Jile :S9 823 09 #1-569 Acq:18-APR-1998 14:27
443.7399 F:4 BSUB(256,30, -3 .0) PKD(7,5,3,
TRIANGLE LABS Text:TLI#45399 M23-FB-3
1003
901
a ol
701
601
sol
401
301
201
101
36:00 37:00 381-00
File:S982309 #1-569 Acq:18-APR-1998 14:27
430.9729 F:4 Exp:NDB5US
TRIANGLE LABS Text:TLI#45399 M23-FB-3
1004 35:52
iyivrVv.. 36:39 37:36 3g:11
soi *^^*^V^v/X"-/vv*'w\Vfc^
80J
70j
60J
50J
401
301
201
j n :
A l/_
0-
36:00 37:00 38.' 00
file:S982309 #1-569 Acq:18-APR-1998 14:27
513.6775 F:4 Exp-.KDBSUS
TRIANGLE LABS Text : TLI#45399 M23-FB-3
1004
90J
80J
70J
601
SO-
' 36:32
:30 EI+ Voltage SIR 70S Noise: 5%
0.05\,20a.O,1.00\,T,T) Exp:NDB5US
INJ-. TIME - 14*30
-2.5E4
.2.21:4
.2.0E4
.1 . 714
.1 . 5£T4
.1.2E4
.9.8E3
17.4E3
.4.9E3
.2.5E3
39:00 40 : 00 41:00 42:00 ' TiJie
:30 EI+ Voltage SIS 70S Noise: 51
0 . 05%,204 .0,1. 00%, J1, T) Exp:HDB5DS
INJ. TIME - 14:30
1 . 8E4
A806.20
-nil'-*- - ^^J^»
.1 . 6E4
.1 . 4E4
.1.3E4
.1 . 1E4
.9 . OE3
.7.2E3
-5.4E3
.3 . 6E3
.1 . 8E3
39:00 40:00 41:00 42:00 Tine
.-30 EI+ Voltage SIR 70S
INJ. TIME =14:30
38:36 39:14 40:25 41-00
KxJ\Nu/vA/.A/\rV'WvVA^i? 3 /L 1 jAA/l Ji/\. 41:37 42: 06 i^
-m if vyv -v v^y^^i^^^^y-vifv^Y ' V^\JUwyWyv^j^\/Vv^
4.2E5
13 . 8E5
.3.4E5
-.3 . OE5
L2.5E5
i2.1E5
Ll . 7£5
.1 . 3£5
L8.51T4
L4.2Z4
39:00 40:00 41:00 42:00 Tine
:30 EI+ Voltage SIR 70S
IlfJ". TIME =- 14:30
3. 9E3
40-j 1 1 38:28
30JI 35:55 1 J 37.54
'• it .j/U \ li P7:01 _ . »M 1
2 0 1 ""»'sJvW*fcAM*--w^W^V\A/^Vv/vJL/V^
JOj
0
36:00 37.- 00 38:00
1 39:39 I i
I . 39:08 1 /, f 40L44\ 41:12 42:i08 1
JW^Ll^yy^yi..*..^ J^w_^.j*.^y\Jl yWiuJi ijAkji Iji JrLjUli ^uJl
.3.5E3
i 3 1E3
'•2.7E3
•-2.4E3
12.0E3
Ll . 6E3
'.1.2E3
.7.BE2
.3.912
39\00 40:00 41:00 42:00 Tine
-------
'i.lesSS82309 #1-569 Acq: 18-APR-I998 14:27:30 EI+ Volt*y* SIS 70S Noiae:42
57.7377 F:4 BSUB(256,30, -3.0) PKD(7,5,3,0.051,168.0,1.00\,F,T) ExpsUDBSOS
TRIANGLE LABS Text:TLI#45399 M23-FB-3 ZKT. TIMX - 14:30
00% A1.70E3
40-36 40:42 40:48 40:54 41:00 41:06
File:S982309 #1-569 Actj:18-APR-1998 14:27:30 11+ Voltage SIX 70S Hoiae:48
59.7348 F:4 BSUB(256,30,-3.0) PKD(7,5,3,0.051,192.0,1.00\,F,T) ExpsKDBSOS
TRIANGLE LABS Tezt:TLI#45399 M23-FB-3 IKT. TIKE - 14:30
40 36 40:42 40:48 40:54 41:00 41:06
File:S982309 #1-569 Acq:18-APR-1998 14:27:30 EI+ Voltage SIR 70S Noi.Be-.38
469.7779 F:4 BSUB(256,30,-3.0) PKD(7, 5,3, 0. 05*,152. 0,1. 00*,F,T) Exp-.JWBSDS
TRIANGLE LABS Text:TLI#45399 M23-FB-3 INJ. TIME - 14:30
A1.20E6
41:12
1003
so:
601
40:
201
A3.22E3
A776.45
41:12
40-36 40:42 40:48 40:54 41:00 41:06
F±le:S982309 #1-569 Acq:18-APS-1998 14:27:30 EI+ Voltage SIS 70S Noise:35
471.7750 F:4 BSaB(256,30,-3:0 ) PKD(7,5, 3, 0. 05%, 140. 0, 1. 00\,T, T) Ezp:NDB5US
TRIANGLE LABS Teit:TLI#45399 M23-FB-3 JM7. TIME = 14:30
1004 A1.4_1E6
41:12
40:36 40:42 . 40:48 40:54 41:00
FilesS982309 #1-569 Acq:18-APR-1998 14:27:30 EI+ Voltage SIR 70S
430.9729 Fs4 Exp:m>B5VS
TRIANGLE LABS Text:TLI#45399 M23-FB-3 ISJ. TIME
1001
41:06
41:12
14:30
1.1E3
9.1E2
6.8E2
4.5E2
2.3E2
.O.OEO
Time
.5.1E2
.4.1E2
.3.1E2
.2.1E2
.1. OE2
.O.OEO
Tine
.1.2E5
.9.2E4
.6.9E4
.4.6E4
.2.3E4
.O.OEO
Time
1.3E5
1.1E5
8.0E4
5.3E4
2.7E4
O.OEO
Tin
^ ^
*
\36 40\42 ' -. ~40\48 40\54 ' ¥lsOO 41\06 ' ' ' Vis 12
^ 3.11:5
12.3B5
11 . 6E5
'.7.8E4
0 . OEO
Time
-------
188 I
838 H
238 9
838 j
818 3
918 0
988 3
W8 8
882 «
-------
10
File:S982309 #1-569 Acq:18-APR-1998 14:27:30 EI+ Voltage SIR 70S
457.7377 F:4 Exp:NDB5US
Sample Text :TLI#45399 M23-FB-3 INJ. TIME =
40:56
14:30 File Text:TLI#45399 M23»
_1.9E3
40:00 41:00
File:S982309 #1-569 Acq: 18-APR-1998 14:27:30 EI+ Voltage SIR 70S
459.7348 F:4 Exp:NDB5US
Sample Text:TLI#45399 M23-FB-3 INJ. TIME =
100%
42:00
Time
14:30 File Text:TLI#45399 M23»
_1.5E3
40:00
4ioo
4200
L7.5E2
L6.0E2
L4.5E2
L3.0E2
Ll.5E2
O.OEO
Time
-------
TLI Project: 45399
Client Sample: M23-RB-1-4
Method 23 PCDD/PCDF Analysis (a)
Analysis File: S982310
Client Project:
Sample Matrix:
TLI ID:
Sample Size:
Dry Weight:
GC Column:
r012.002/Lime Kiln
M23
204-92-12A-D
1.000
n/a
DB-5
Date Received:
Date Extracted:
Date Analyzed:
Dilution Factor
Blank File:
Analyst:
04/01/98
04/03/98
04/18/98
n/a
U980780
DL
Spike File:
ICal:
ConCal:
% Moisture:
% Lipid:
% Solids:
SPMIT204
SF51078
S982303
n/a
n/a
n/a
>**%&?&
% \ f*v % % t % 5>^X"b ^ +* "* NXv>?tiv**\ %v
2,3,7,8-TCDD N
1,2,3,7,8-PeCDD N
1,2,3,4,7,8-HxCDD N
1,2,3,6,7,8-HxCDD N
1,2,3,7,8,9-HxCDD is
1,2,3,4,6,7,8-HpCDD h
U,3,4,6,7,8,9-OCDD N
2,3,7,8-TCDF h
1,2,3,7,8-PeCDF ^
2,3,4,7,8-PeCDF h
lA3,4,7,8-HxCDF h
1^,3,6,7,8-HxCDF h
2,3,4,6,7,8-HxCDF ^
1,2,3,7,8,9-HxCDF h
1,2,3,4,6,7,8-HpCDF ^
1^,3,4,7,8,9-HpCDF ^
1A3,4,6,7,8,9-OCDF ^
Totals x_;s,;; , \ ;ul;A*
Total TCDD h
Total PeCDD ^
Total HxCDD ^
Total HpCDD 1>
Total TCDF h
Total PeCDF h
Total HxCDF t
Total HpCDF I
Cv« % •*. -y- 3?? w^®3S^^^^^^ F$8Jj$:$&y''&& '$$$$8$§%$$§i9FQ^'v ? \&$$S§t$$§&8$& ^^^^tS^^»^^^^®SSwll^^^^3
ID 0.003
ID 0.004
ID 0.004
ID 0.004
ID 0.004
ID 0.004
ID 0.005
ID 0.002
ID 0.003
ID 0.003
ID 0.003
ID 0.003
ID 0.003
ID 0.003
ID 0.003
ID 0.004
ID 0.004
. (ftgp^ifcjnitfcr 'Bfc m?v \\^-^-r^^'^^\^^^^^,f
ro o.oo3
tt> 0.004
ID 0.004
ID 0.004
4D 0.002
•ID 0.003
rt> 0.003
«ID 0.004
Page 1 of 2
ionJ>SR »IM. LARS 6.11 DO
Triangle Laboratories, Inc.®
801 Capitola Drive • Durham, North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 20:28 04/20/9
-------
TLI Project: 45399
Client Sample: M23-RB-1-4
Method 23 PCDD/PCDF Analysis (a)
Analysis File: S982310
l3Ci2-2,3,7,8-TCDF
13Ci2-2,3,7,8-TCDD
l3C,2-l,23,7,8-PeCDF
13Ci2-l,2,3,7,8-PeCDD
l3Ci2-l,23,6,7,8-HxCDF
l3C,2-l,2,3,6,7,8-HxCDD
'3C,2-l,23,4,6,7,8-HpCDF
I3C12-l,2,3,4,6,7,8-HpCDD
'3Ci2-1.2,3,4,6,7,8,9-OCDD
2.6
2.4
2.5
3.0
33
3.9
3.3
4.0
9.2
66.0
59.9
62.5
76.1
81.6
97.6
82.8
101
115
40%-130%
40%-130%
40%-130%
40%-130%
40%-130%
40%-130%
25%-130%
25%-130%
25%-130%
0.71
0.80
1.57
1.48
0.50
1.21
0.42
1.01
0.85
25:14
25:57
29:10
30:13
32:44
33:27
35:44
36:52
40:42
13C,2-2,3,4,7,8-PeCDF
13C12-l,2,3.4,7,8-HxCDF
'3C,2-1.2,3,4,7,8-HxCDD
'3Ci2-1.2,3,4,7,8,9-HpCDF
4.0
3.3
3.3
3.8
101
82.5
82.5
95.2
40%-130%
40%-130%
40%-130%
25%-130%
1.53
0.50
1.20
0.43
29:52
32:38
33:22
37:22
"CU-^J.S-TCDD
3.4
83.8
40%-130%
25:58
Arat
13Ci2-1.2,3,7,8,9-HxCDF
13Ci2-2,3.4,6.7,8-HxCDF
3.5
3.6
87.7
89.1
40%-130%
40%-130%
0.51
0.50
34:03
33:15
Recovery Slanctarrfs
Ratio
13C12-1,2,3,4-TCDD
'3C,2-l,2,3,7,8,9-HxCDD
0.79
1.19
25:46
33:47
Data Reviewer
Page 2 of2
04/20/98
Hmj-SR »|J04. LARS 6.11.00
Triangle Laboratories, Inc.®
801 Capitola Drive • Durham, North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 20:28 04/20/98
359
-------
Initial
Date..
Data Review By:
Calculated Noise Area:
0.10
The Total Area for each p«ak with an ion abundance ratio outside
ratio limits has been recalculated according to method requirements.
Page No.
04/20/98
Listing of S982310B.dbf
Matched GC Peaks / Ratio / Ret. Tine
Compound/
H_Z QC.Log Omit Vftiy ..RT. OX Ratio Total.Area... Area.Peak. 1.. Area.Peak.2.. Rel.RT Compound.
Ham*.. ID.. Flags.
TCDF
304-306
304-306
13C12-TCDF
316-318
316-318
TCDD
320-322
D
320-322
37C1-TCDD
328
328
13C12-TCDD
332-334
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
d
DC
DC
DC
NL
0
NL
ML
WL
4
NL
SN
SN
SN
SN
SN
SN
SN
SN
SN
SN
0
0:00
Peaks
0:00
23:15
24:12
24:31
24:50
25:14
25:40
Peaks
0:00
23:26
23:34
23:43
23:53
24:12
24:26
24:46
25:30
25:44
25:59
Peaks
0.
RO
0.
RO
RO
0.
RO
RO
RO
RO
RO
RO
RO
RO
RO
65-0.89
1.
23
0
0
.23
.00
65-0.89
1.
1.
0.
0.
0.
0.
0.
00
46
71
88
71
71
86
0
0
12
1
3
434
1
440
tHf*TV
.28
.42
.07
.05
.00
.08
.90
.03
D / m^n
65-0.89
0.
4.
0.
0.
0.
0.
0.
1.
1.
3.
0.
90
00
43
67
40
83
18
00
20
75
37
0
0
0
0
0
0
0
0
0
0
0
0
.18
.04
.07
.10
.05
.11
.07
.39
.09
.07
.16
.00
0.873-1.075
0
.000
0.960-1.040
0
0
0
0.49 0.56 0
1.25 1.75 0
180.06 254.02 1
0.88 1.02 1
.000
.921
.959
.972
.984
.000 13C12-2378-TCDF
.017
ISO
0.899-1.046
0
0
0
0
0
0
0
0
0
0
1
.000
.903
.908
.914
.920
.933
.942
.954
.983
.992
.001 2378-TCDD
AN
0.923-1.077
DC
DC
DC
NL
SN
4
NL
0:00
24:35
25:07
25:58
26:10
27:27
Peaks
0:00
24:46
25:46
25:57
0.
RO
RO
0
1
0
240
0
0
242
.13
.40
.12
.64
.28
.16
.48
65-0.89
1.
0.
0.
0.
27
94
79
80
0
1
458
302
.27
.54
.13
.52
0
1.40 0
0
240.64 1
0.28 1
0.16 1
.000
.947
.968
.001 37C1-TCDD
.008
.058
CLS
0.923-1.077
0
0.82 0.87 0
202.61 255.52 0
134.10 168.42 1
.000
.954
.993 13C12-1234-TCDD
.000 13C12-2378-TCDD
RSI
IS1
Triangle Laboratories, Inc.® Analytical Services Division
801 Capitals Drive • Durham. North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 20:28 04/2CV98
- 360
-------
Page No.
04/20/98
Listing of S982310B.dbf
Matched QC Peak* / Ratio
/ Ret. Tine
Cocqpound/
M_Z QC.Lofl Omit Why ..RT. OK Ratio Total. ATM.. . ATM.Peak. 1.. Area.Peak.2.. Rel.BT Coaeound.HaiM.. ID.. Flags.
332-334
FeCDF
340-342
340-342
13C12-PeCDF
352-354
352-354
PeCDD
356-358
356-358
13C12-PBCDD
368-370
368-370
HxCDF
374-376
26:17
4 Peaks
0.89
1.32-1.78
DC ML 0:00 RO 1.00
DC SN 29:20 1.75
DC SM 29:30 RO 0.17
DC SN 29:39 RO 0.50
DC SM 29:45 RO 0.60
DC SN 29:54 RO 0.73
DC SN 30:08 RO 0.38
0 Peaks
1.32-1.78
DC ML 0:00
28:19
28:47
29:10
29:20
29:27
29:52
30:14
30:49
8 Peaks
DC NL 0:00
DC SN 29:37
DC SM 29:49
0 Peaks
DC ML 0:00
29:07
29:17
30:13
30:20
DC SM 30:45
4 Peaks
DC ML 0:00
DC SN 31:50
DC SM 32:15
DC SN 32:20
DC SN 33:02
RO
RO
RO
RO
RO
1.
RO
RO
RO
1.
1.
1.
1.
0.
1.
1.
1.
1.
11
51
80
57
89
34
53
09
00
ftluHM. .
4.44 2.09
766.63
0.13
0.11
0.12
0.05
0.10
0.13
0.05
0.00
0.
18.
0.
308.
1.
2.
301.
0.
0.
633.
16
55
89
06
28
78
10
41
92
99
11.
0.
188.
0.
1.
182.
0.
0.
15
63
06
78
59
19
25
56
2.35
1.013
0.928-1.063
0.000
1.006
1.011
1.017
1.020
1.025 23478-PeCDF AH
1.033
0.863-1.137
7.40
0.35
120.00
0.88
1.19
118.91
0.23
0.56
0.
0.
0.
1.
1.
1.
1.
1.
1.
000
971
987
000 13C12-PeCDF 123 IS2
006
010
024 13C12-PeCDF 234 SOR1
037
057
32-1.78
1.
00
2.00
1.22
0.937-1.022
0.13
0.13
0.18
0.000
0.980
0.987
0.00
1.
RO
RO
RO
32-1.78
0.89
1.00
2.74
1.48
1.44
RO
1.
RO
RO
RO
RO
RO
2.11
0.
0.13
0.48
0
208
17
0
226
•n**.f*n'
,05-1.43
0
2
0
0
1
.90
.00
.67
.33
.50
0
0
0
0
0
.59
.19
.71
.23
.97
n / Uvt
L* / roc*
.16
.16
.04
.02
.04
0.29
0.63
124
10
.24
.45
0.29
0.23
83.95
7.26
868-1.132
0.000
0.964
0.969
1.000 13C12-P«CDD 123 IS3
1
1
.004
.018
0.
963-1.048
0
0
0
0
1
.000
.973
.985
.988
.009
Triangle Laboratories, Inc.® Analytical Services Division
801 Capitals Drive • Durham. North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 20:28
04/20/9$ t
-------
Pag* No. 3
04/20/98
Confound/
M_Z.... QC.Log Omit Why
Listing of S982310B.dbf
Matched OC Peaks / Ratio / Ret. Tiaw
-RT. OK Ratio Total. Area... Area.Peak.1.. Area.Peak.2.. Rel.BT CoBpound.lIane.. ID.. Flags.
374-376
13C12-HXCDF
384-386
384-386
HXCDD
390-392
D
390-392
13C12-HXCDD
402-404
402-404
HpCDF
408-410
D
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
d
DC
DC
DC
DC
DC
DC
DC
DC
DC
d
SN
HH
WH
0
NL
SN
SN
SN
SN
8
NL
SN
SN
SN
SN
SN
SN
SN
SN
SN
0
NL
6
NL
SN
SN
33:05
34:34
34:38
Peaks
0:00
31:40
31:47
32:38
32:44
32:58
33:01
33:03
33:15
33:29
33:32
34:03
34:22
Peaks
0:00
32:26
32:34
32:38
32:43
32:49
32:58
33:03
33:09
33:17
Peaks
0:00
32:50
33:22
33:27
33:47
34:01
34:13
Peaks
0:00
35:50
35:55
RO
RO
0.
RO
RO
RO
RO
RO
RO
RO
RO
1.
RO
RO
RO
RO
RO
RO
RO
RO
1.
RO
RO
RO
0
I RO
1 RO
1.38
0.40
3.50
43-0.59
0.87
0.60
0.54
0.50
0.50
0.23
0.27
0.18
0.50
0.42
0.69
0.51
0.67
1
05-1.43
1.29
3.00
1.00
1.00
2.13
1.20
0.60
0.70
0.75
2.44
,05-1.43
1.56
1.46
1.20
1.21
1.19
1.39
1.94
.88-1.20
0.81
2.75
0.90
0.19
0.04
0.04
0.00
0.23
3.47 1.37
6.79 2.39
254.40 84.46
303.42 101.46
0.18
0.09
0.18
327.85 109.60
0.56 0.19
0.20
259.19 87.04
0.32 0.14
.156.00
0.16
0.04
0.07
0.25
0.18
0.22
0.05
0.13
0.05
0.20
0.00
0.20
1.57 1.02
199.35 108.74
262.94 143.85
291.63 158.76
0.86 0.50
0.38 0.33
756.73
HxCDD / HpCDF Follows — — •
0.26
0.08
0.40
1.011
1.056
1.058
0.878-1.122
0.000
2.30 0.967
4.40 0.971
169.94 0.997 13C12-HXCDF 478
201.96 1.000 13C12-HXCDF 678
1.007
1.009
1.010
218.25 1.016 13C12-HXCDP 234
0.45 1.023
1.024
172.15 1.040 13C12-HXCDF 789
0.21 1.050
0.958-1.014
0.000
0.970
0.974
0.976
0.978
0.981
0.986
0.988
0.991
0.995
0.970-1.030
0.000
0.70 0.982
90.61 0.998 13C12-HXCDD 478
119.09 1.000 13C12-HXCDD 678
132.87 1.010 13C12-HXCDD 789
0.36 1.017
0.17 1.023
0.997-1.051
0.000
1.003
1.005
SOR2
IS4
ALT2
ALT1
SUR3
IS5
RS2
Triangle Laboratories, inc.® Analytical Services Division
801 Capitola Drive • Durham, North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 20:28 04(00/98
-------
Page Mo.
04/20/98
Lilting of S982310B.dbf
Matched OC Peaks / Ratio
/ R«t. Tine
Compound/
M_Z OjC.Log Omit Why . .RT. OK Ratio Total.Area... Area.Peak.1.. Area.Peak.2.. Rel.FT Caapound.Hame.. ID.. Flag*.
408-410
0 Peaks
0.00
13C12-HpCDF
418-420
0.37-0.51
DC
ML
0:00 RO
35:44
36:07 RO
418-420
HpCDD
424-426
424-426
13C12-HpCDD
436-438
436-438
OCDF
442-444
442-444
OCDD
458-460
458-460
13C12-OCDD
470-472
470-472
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
3
ML
SN
SN
0
ML
2
ML
HL
SN
SN
SN
SN
SN
SN
SN
SN
SN
0
ML
SN
SN
SN
SN
SN
0
ML
37:22
Peaks
0:00
36:13
37:02
Peaks
0:00
36:04
36:52
Peaks
0:00
36:37
37:50
37:55
38:01
38:38
38:43
38:50
39:08
39:15
39:18
Peaks
0:00
40:41
40:54
40:54
41:06
41:12
Peaks
0:00
40:42
0.
RO
RO
RO
0.
0.93
0.42
0.95
0.43
ktuM*m •
88-1.20
1.25
4.50
0.67
88-1.20
1.14
0.94
1.01
0.22
204.45 60.09
0.
155.
360.
0.
0.
0.
0.
0.
2.
32 0.21
83 46.84
60
i / UW"nn Vnl 1 j-imM ..
/ np<*isu roAAowa ~*
16
04
08
00
30
41 1.17
217.46 109.39
0.944-1.112
0.000
144.36 1.000 13C12-1&CEF 678
0.22 1.011
108.99 1.046 13C12-HpCDF 789
0.976-1.005
0.000
0.982
l.OOS
0.973-1.027
0.000
1.24 0.978
108.07 1.000 13C12-HpCDD 678
IS6
SDR4
IS7
219.87
0.
RO
RO
RO
RO
RO
RO
RO
RO
RO
RO
0
RO
RO
RO
RO
RO
0
RO
_ ft VvntK •
76-1.02
1.00
0.75
0.75
3.50
1.67
0.40
2.00
0.19
0.71
0.10
0.31
.76-1.02
1.00
6.50
0.75
0.43
0.50
0.50
.76-1.02
1.13
0.85
1 Peak
tlWTW
npt»ui
0.16
0.19
0.13
0.04
0.17
0.04
0.09
0.06
0.11
0.02
0
0
0
0
0
0
0
0
0
.08
.00
.16
.04
.06
.06
.08
.02
.00
0.15
337
337
.69 154.89
.69
0.902-1.098
0.000
0.900
0.930
0.932
0.934
0.949
0.951
0.954
0.962
0.964
0.966
0.902-1.098
0.000
1.000 OCDD
1.005
1.005
1.010
1.012
0.996-1.004
0.000
182.80 1.000 13C12-OCDD
AN
IS8
Triangle Laboratories, Inc.® Analytical Services Division
801 Capftola Drive • Durham, North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 20:28 04/20/98
363
-------
Page No.
04/20/98
Listing of S982310B.dbfi
Matched GC Peak* / Ratio / Ret. Time
Compound/
M_Z ____ QC.Log Omit Why . .RT. OK Ratio Total. Area. .. Area. Peak. 1. . Area. Peak. 2. . Rel.RT Compound. Kane. . ID.. Flags.
Column Description
'Wiy- Code Description ......... QC Log D«sc.
M_Z -Nominal Ion Mass(es)
..RT. -Retention Tine (nntss)
Rat.l -Ratio of M/M+2 Ions
OK -RO»Ratio Outside Limits
Rel.RT- Relative Retention Tine
End of Report
ML- Below Retention Tins Window
HH-Above Retention Tims Window
SM-Below Signal to Noise Level
-------
rile
303. <
TRIM
100]
so:
60:
40.
20.
0
rile
305.
TRIA.
100]
aoj
60:
40:
20:
0
rile
315.
TRIA.
100]
80:
sol
40:
20:
0
rile
317.
TRIA
1001
80:
so:
40:
20:
b:
rile
330.
TRIA
1001
sol
sol
40.
20.
0
tilt
375.
TRIi
100]
80.
60.
40.
20.
0
r 5982310 tl-746 AcqtlS-APR-1998 15:13:36 XI* Voltage SIR 70S Btoim»i78
1016 Ts2 BSUB(2S6,30,-3.0) rXD(9, 5, 5,0. 051,312. 0,1.00\,r,T) XxptHDBSOS
VGLE LABS Tmxt>TLI«45399 M23-RB-1-4 HU. TIME - 15:16
A2.74E3
1 A1.30E3
1 I I JA1.25X3
'23(00 ' 24(00' ' ' 25*00 ' '20(00 27(00'
IS982310 tl-746 Acq:18-APR-1998 15:13:36 XI* Voltage SIR 70S Koim»:63
8987 T:2 BSVB(256,30, -3.0) fH)(9,5,5,0.05\,252.0,1.00\,T,T) XxptNDBSOS
HGLE LABS Zext( 3X1*45399 M23-RB-1-4 IKT. TIME * 15(10
A4. 2X3
• I
A2.99X3 II ill
/K%^
'23(00 '' ' 24sOO ' 25»00 26:00 27(00'
.•5982310 tl-746 Acq:18-APR-1998 15(13(30 XI* Voltage SIR 70S Koiae:81
9419 Tt2 BSUB(256,30,-3.0) PKD(9,5,5,0 .05\,324 .0,1.00\,r,T) Exp:NDB5US
HGLE LABS T«xtiTLIt45399 M23-U-1-4 XK7. TIME - 15(16
A1.80E6
11
23:00 .• 24:00 25:00 26:00 27:00
.•5982310 #1-746 Acq:18-APR-1998 15:13:36 EI+ Voltage SIS 70S Boi*e:78
9389 Fi2 BSOB(256,30,-3.0) PKD(9, 5, 5,0. 051,312. 0,1.00\,r,T) ExpiKDBSOS
OGLE LABS Text:TLH45399 M23-RB-1-4 JK7. TIKE • 15:16
A2.54E6
|
'
11
23:00 24:00 25:00 26:00 27:00
-.3962310 tl-746 Aoq:18-ATR-1998 15:13(36 EH- Voltage SIS 70S
9792 Tt2 ExpsSDBSUS
MGLE LABS Text : TLIM5399 M23-JIB-1-4 UW. TIME - 15:16
h~^#-^C^^^ — ^^A^i^iL-^^^Jj^
23:00 ' 24:00 ' ' 25(00 26:00 ' 27\00~
t:5982310 fl-746 Acq:18-APX-1998 15(13:36 XI* Voltage SIS 70S
8364 Fi2 Exp:KDB5US
INGLE LABS Text : 2X1*45399 H23-RB-1-4 IJKT. TIME - 15:16
22:41 35>°4 1
~^d^J(w£w^
23:00 24:00 25(00 26(00 27(00
.1.0X3
.•.3X2
.6.2X2
.4.1X2
-2.1X2
•0.0X0
.1.2X3
.1.0X3
.7.5X2
.5.0X2
.2.5X2
0.0X0
-5.2X5
.4.2E5
L3.1X5
L2.1X5
11.0X5
•o.oxo
r7.3X5
.5.8X5
.4.4X5
.2.9X5
.1.5X5
0.0X0
Time
1.1X6
.8.5X5
.6.4X5
.4.2X5
.2.1X5
0.0X0
Ti*e
-1.8X3
111.4X3
11.1X3
.7.1X2
L3.5X2
0.0X0
36
-------
Filet S982310 #1-745 Acg:lfl-APX-Z998 15*13*35 EH- Voltmgm SIX 70S Hoi**: 43
319.8965 F:2 BSUB(256,30,-3 .0) PO>( 7,5, 3,0. 051,172.0, 1.00\,r,T) Xxp:KDB5OS
TRIANGLE LABS Tart »TX,X #45399 M23-SB-1-4 XKT. TIME - 15*15
1001
80:
50:
40:
20:
A2.18£3 A
I
A1.1SX3 I 1
1 1 It 1
24(00 25*00 25*00
Flla:S982310 #1-745 Acg«lfl-APB-1998 15*13*35 EH- Voltmgm SIX 70S
_7.5r2
2.79£3
1 A1.57X3
A5fi'°5 I
i^Uvw^^
L«.1X2
14.6X2
.3.lX2
.1.5X2
27* 00 Time
Hbi»mt52
321.8936 Fi2 BSUB(256,30,-3.0) PKD(7,5,3,O.OS\,20B.O,1.00\,F,T) XxpsXDBSUS
TRIANGLE LABS Jflftrt « TLIf 45399 M23-SB-1-4 XKT.
100J
80:
50:
40:
0.
A626.47 A1.87X3
Jj-
*
ma • 15*15
-9.4X2
r .tryt'vf>(.0^l ^"' °
Mi. S9 823 10 #1-745 Acq-*18-Al>JR-1998 15*13*35 EH- Voltagw SXX 70S
330.9792 Ft 2 ExpsHDBSUS
TRIANGLE LABS T«xt » IZX#45399 M23-XB-1-4 XKT.
100J
80.
50.
40J
20J
OJ
TIME - 15:15
5.7r5
-.5.3X5
.4 . 0X5
.2.7X5
-1.3E5
27*00 Tjjie
TTMT - 15*16
^^^^^ii^i^iios^^j^
*•
24*00 25*00 25*00
-1.1X6
.8.5X5
.6.4X5
.4.2X5
.2.1X5
27,00 Ti.«
366
-------
ile:S982310 tl-746. AcqilB-AfX-1998 15:13:36 XI+ Voltage SIX 70S Hoimei39
39.8597 r*2 BSUB(256,30,-3.0) PKV(7,5,3,0.051,156.0,1.00\,r,T) XxpiNDBSffS
TRIANGLE LABS Teit*TLIt45399 M23-XB-1-4 XXT. TIMS - 15tiff
OOS
28:00 39i00 30i00
•He: 39 82310 tl-746 Acq:18-APX-1998 15.13.J5 JJ+ Voltage SIX 708 Boise:41
341.8567 ri2 SSUf(256,30,-3.0) HfD(7,5,3,0.05%, 164.0,1.00\,f,T) XipiXDBSUS
TXIMKLS TABS T«xt:ZLJ*45399 M23-XB-1-4 OKT. XZKE -
1004 A4.J.3X3
28:00 . 29.00 30.00
rilasS9B2310 tl-746 Aoq>18-APX-1998 15:13:36 XI+ Voltage SIX 708 Hoit»>49
351.9000 Tt2 BSUB(256,30*-3.0) PXD(7,5,3,0.051,196.0,1.00\,r,T) SxptXOBSUS
TBIANSLX LABS T»xt:TLIt45399 H23-XB-1-4 XKT. TIMS - 15:16
ion
aol
601
40:
20J
31100
31 i 00
20.00 29.00 JO.00
J-il«!S982J10 tl-746 AcqilB-AfX-1998 15:13:36 EH- Voltage SIX 70S Boii»t44
353.8970 F:2 BSUB(256,30,-3.0) PKD(7,5,3,0.05\,176.0,1.00\,T,T) SxptUDBSUS
TXIAHSLS LABS TmxtiTLIt45399 M23-XB-1-4 B&. TIMS - 15:16
SltOO
1001
sol
50:
40:
20:
A1.20E6
28:00 29.00 JO*00
riletS9B2310 tl-746 Acq:18-APX-1998 15.1J.J5 EH- Voltage SIX 70S
330.9792 F:2 SxptSDBSUS
TRIANGLE LABS Text i XLIt45399 M23-XB-1-4 IMJ. TIME -
Jl.-OO
15.16
iota
80:
50:
40:
20:
27:20
27:44
28:15
28:00 29.00 JO:00
J-11..5982J10 #1-746 Aoj:18-AP*-1998 15:1J.J6 JET* Voltage SIX 70S
409.7974 Tt2 ExpiNDBSOS
TXIAHSLE LABS TextiTLIt45399 M23-XB-1-4 UKT. TIME -
15:15
31:00
Jl 02
Time
7.8X2
6.3X2
4.7X2
3.1X2
1.6X2
.0.0X0
Time
5.7X5
4.6X5
3.4X5
2.3X5
1.1X5
0.0X0
Time
3.8X5
3 . 0X5
2.3X5
1.5X5
7.6E4
O.OEO
Tim
.1.1X6
.8.7X5
.6.5*5
.4.425
.O.OEO
Time
^1.8X3
28100
29 tOO
30:00
31:00
-------
91-746 Acq:lB-APX-l998 15,13,36 g+ Voltage 31* JOS 9oi,e:JB
355.8546 Tt2 BSOB(2S6,30, -3.0) PKD(7,5,3,0.05\t152.Q,1.0Q\,r,T) Ezp:lO>B5US
TRIANGLE LABS Text:TLIf 45399 M23-XB-1-4 OJ. TIME - 15s 16
lOOi, A2.20E3
J I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I
28:24 28:36 28:48 29iOO 29:12 29:24
Tile:S982310 fl-746 Acqtl8-APX-1998 15:13*36 El* Voltage SIX 70S Holme:39
357.8516 T:2 BSUB(256,30,-3.0) PKD(7,5,3,0.05\,156.0,1.00\,T,T) ExptUDBSUS
TRIANGLE LABS Text :TLIf 45399 M23-XB-1-4 XK7. TIME - 15:16
1004
28124 28:36 28:48 29:00 29:12 29:24 29:36 29:48 30:00 30:12 30:24 30:36 30:48 31:00 31:12
Tile:S982310 fl-746 Acqsl8-APK-1998 15:13:36 EL+ Voltage SIX 70S Boiae:42
367.8949 Tt2 BSUB(256,30,-3.0) PKD(7,5,3,0.05\,168.0,1.00\,r,T) XxpiHDBSUS
TRIANGLE LABS Toxt:TLI*4S399 M23-SB-1-4 UKT. TIME - 15:15
1003k A1.24E6
so:
60.
40.
20.
OSES
28:24 28:36 28t48 29:00., 29:12 29:24 29:36 29:48 30:00 30:12 30:24 30:36 30:48 31:00 31:12
File:3982310 fl-746 Acq:18-APR-1998 15:13:36 EI+ Voltage SIS 70S Ko±m»:44
369.8919 1:2 BSUB(256,30;-3.0) PKD(7,5,3,0.05\,176.0,1.00\,T,T) ExptNDBSOS
TRIANGLE LABS Text:TLI*45399 H23-RB-1-4 UKT. TIME - 15»1«
100J
80.
60.
40.
20.
A8.40E5
7.26E4
28:24 28:36 28:48 29:00 29:12 29:24 29:36 29:48 30:00 30:12 30:24 30:36 30:48 31:00 31:12
Tlle,S982310 fl-746 Acq:18-APX-1998 15:13:36 EH- Voltage SIX 70S
330.9792 T:2 Exp:NDB5US
TRIANGLE LABS Teit:TLIt453S9 M23-RB-1-4 HUT. TIME * 15:16
ion
80.
SOL
40.
20.
0.
29: 20
r-J-
28:24 28:36 28:48 29:00 29:12 29:24 29:36 29:48 30:00 30*12 30:24
30>48 3l':6o' 31:12
OSO
Time
.OE5
.2E5
.4X5
.6ES
.9E4
.OEO
Time
.7ES
,2E5
.6E5
.1E5
.4E4
.OEO
Time
1E6
7E5
6E5
4E5
2ES
OEO
Time
368
-------
±1»*S982310 fl-465 Aoq*18-APX-1998 15*13*36 EH- Volt*y» SIX 70S moimm*44
73.8208 fi3 BSUB(256,30,-3.0) FXD(7,5,3,0.05\,176.0,1.00\rr,T) ExpiXDBSOS
TXIA1KLE LABS Tuxt*TLH45399 M23-XB-1-4 IJKT. TIME - 15.15
00\A530.26
31*36 31*48 32*00 32*12 32*24 32*36 32*48 33*00 33*12 33*24 33*36 33:48 34*00 34*12 34*24 34*36
•il»: 39 82310 11-465 Acq:18-APR-1998 15*13*36 EH- Voltage SIX 70S Ooimui48
375.8178 Ts3 BSUB(256,30,-3.0) tKD(7,5,3,0.05\,192.0,1.00\,r,T) ExptMDBSUS
TRIANGLE LABS T
-------
>il*,S9B33lO U-465 Aoy,l8-AfX-l99B IS,13,JS fl* Volfaig* Sit JOS Ooim»,44
89.8156 Tt3 3803(256,30,-3.0) Pja>(7,5,3,0.05\,176.0,1.00\,r,T) XxptNDBSUS
TRIANGLE LABS T*xt,TLIt45399 H23-RB-1-4 IW. TIME " 15il6
001 A2.22E3
37:12
32i24 32,36 32,48 33,00 33il2 33*24 33i36 33,48
ttlf,S982310 tl-465 Acq,18-APX-1998 15113:36 11+ VbJtag* SIM 70S Soim»,36
391.8127 r,3 3803(256,30,-3.0) PXD(7,5,3,0.05\r144.0,1.00\,r,T) X*piHD35OS
TRIABGLX LA38 TvrttTLI*45399 M23-X3-1-4 UKT. HOC - 15tl6
100* A1.02X3
801
60.
40:
20.
34tOO 34112
-r
T
-r
-r
32>12 32t24 32>36 32i48 33iOO 33>12 33i24 33t36 33i48
File:S982310 #1-465 Aoqtia-APX-1998 15,13,36 SI+ Voltage SIB 70S Xoi*»t68
401.8558 r-.3 3SU3(256,30,-3.0) PKD(7,5,3,O.OS\t272.0,1.00\,r,I) SxptSDSSOS
TKIAHSLS LA3S T«xttTLI*45399 M23-R3-1-4 IKf. TDfK " 15>16
1001 A1.59E6
'34',00 ' '34',12
,7.1X2
.5.7X2
.4.3X2
.2.8X2
'.1.4X2
'.0.0X0
Timu
ao:
eo:
40.
20.
A1.44S6
32:12
' 32\24
i
32\36
32s 48
33:00
1
33\12 h's
24 33s 36
33:48
34:00
34:12
.4.1X5
.3.3X5
.2.5X5
.1 . 6X5
.8.2X4
0.0X0
Tile:S982310 tl-465 Acqtia-APR-1998 15sl3:36 EI+ Voltag* SIX 70S Boi*e:43
403.8529 Fs3 3SU3(256,30*-3.0) PKD(7, 5,3, 0.051,172.0,1.00\,r,T) ExptNDBSUS
TBIANGLE LABS T«xtsTLIt45399 M23-RB-1-4 XXT. TIKE " 15tl6
1001 A1.33X6
80.
60.
40.
20.
.3 . 4X5
'.2.8X5
'.2.1X5
.1 . 4X5
.6.9X4
32:12 32\24 ' '32:36 ' '32,48 33tOO 33,12 33,24 33,36 33:48
File:S982310 tl-465 Acq:18-APX-1998 15,13:36 EI+ Voltage SIS 70S
392.9760 r,3 ExpiNDBSUS
TRIANGLE LABS TextiTLIt45399 M23-XB-1-4 IKT. TIME - 15,16
10°* 32,14 32,24 32,37 . 32:52
60.
40.
20.
34,00 34,12
34,08
.0. 0X0
Tim.
.5.4X5
-4.3X5
.3.2X5
.2.2X5
.1.1X5
'32\12 ' '32,24 32,36 32,48 33,00 33,12 33,24 33,36 33,48 34,00 34,12
0.0X0
Tim.
370
-------
'ile,S982310 tl-569 Acqil8-APX-1998 15,13,36 EH- Voltmye SIX 70S Hoif9,64
407.7818 F,4 BSOB(256,30,-3.0) PKD(7,5,3, 0.05\,256.0,1.00\,T,T) XxptHDBSUS
TRIANGLE LABS Text,TLIt45399 K23-XB-1-4 1X7. TIKX - 15:16
1003
80:
60:
40:
20:
o:
35,48 36i00 36,12 36,24 36,36 36,48 37,00 37,12 37,24
ril»:3982310 tl-569 Acq,18-APX-1998 15,13,36 SI+ Volttg* SIX 70S Jk)if»,79
409.7789 tit BSUB(256,30,-3.0) PKD(7,5r3,0.05\,316.0,1.00\,r,T) XxpiXDBSUS
TXIUKLX LABS T*xtsTLIt45399 M23-XB-1-4 ZIK7. TXMX " 15s 15
100*
35,48 36,00 36,12 36:24 36,36 36,48 37,00 37,12 37,24
r±l»,S982310 tl-569 Acqil8-APX-1998 15,13,36 EH- Volt*?* SIB 70S Boi*»,69
417.8253 T:4 BSUB(256,30,-3.0) PXD(7,5,3,0.05\,276.0,1.0Q\,T,T) XzptXDBSUS
TXIAJKLS LABS Text:TLH45399 H23-XB-1-4 HKT. TIME • 15,16
1001A6.01ZS
A1.93S3
A1.13E3
A859.32
/VA^ww^^^
37,36 37,48
80:
60:
40:
20:
A4.68E5
35,48 36,00 36,12 36,24 36:36 36,48 37,00 37,12 37,24
r±l»,S982310 tl-569 Aoqsl8-APR-1998 15,13,36 EH- Voltage SIX 70S Koif»,74
419.8220 f,4 BSOB(256,30,-3.0) PXD(7,5,3,O.OS\,296.0r1.00\,T,T) Exp:XDB5US
TXIJOKLE LABS T»3CtsTLIt4'5399 K23-XB-1-4 HKT. XIHE -
100\A1.44E6
37,36 37,48
80:
60:
40:
20:
0.
Al.09E6
35,48 36,00 36,12 36,24 36,36 36,48 37:00 37,12 37,24
File,S982310 tl-569 Acq,18-APX-1998 15,13,36 EH- Voltaya SIX 70S
430.9729 T,4 SxptKDBSUS
TRIANGLE LABS Text:TLIt45399 M23-KB-1-4 IXJ. TIKE • 15,16
36,53 37,08 37,19
80:
60:
40:
20:
o:
35,48 36,00 36,12 36,24 36,36 36,48 37,00 37,12 37,24
F±1»:S982310 tl-569 Acq,18-APX-1998 15,13,36 EH- Volttge SIX 70S
479.7165 T,4 ExpiHDBSOS
TRIANGLE LABS TeittTLIt45399 H23-KB-1-4 JK7. TIKE « 15:16
1003
80:
60:
40:
20:
o:
_1. 8X3
.1.5X3
.1.1X3
17.4X2
.3.7X2
0.0X0
35,46
36,00
36,12 36,24
36,36
36,48 37,00 37,12 37,24 37,36 37,48
0.0X0
Time
1.2X5
9.7X4
7.3X4
4.9X4
2.4X4
0.0X0
Time
.3.0X5
.2.4X5
.1.8X5
.1.2X5
.5.9X4
.0.0X0
Time
3.6X5
.2.9X5
.2.2X5
.1. 5X5
.7.3X4
.0.0X0
Time
.1. 7X3
.1. 4X3
.1.0X3
6.8X2
.3.4X2
O.OEO
Time
-------
File:398^310 #1-569 Acq,lB-Af*-19S8 J5.lJ.Jg HI Volt*ym Sit 70S Hoi**,51
423.7766 f:4 BSOB(256, 30, -3.0) PKD( 7,5,3,0.05%, 204.0,1.00\,T,T) XzptHDBSUS
TXIAHSLX LABS T*xt,TLH45399 M23-XB-1-4 UKT. TIMS - 15tl6
1001 A2.07E3
36100 36:06 36:12 36:18 36t24 36i30 36t36 36t42 36t48 36t54 37:00 37t06 37il2 37*18
rll»,S982310 fl-569 AcqtlB-APS-1998 15,13,36 EI+ Voltage SIX 70S Boifm:39
425.7737 Tt4 BSUB(256r30,-3.0) PKD(7,5,3,0.05\,156.0,1.00\,T,T) ExpiXDBSOS
TXIAXSLX LABS Text:TLH45399 M23-RB-1-4 OKT. TIMX - 15,16
1001
36,00 36,06 36,12 36,18 36,24 36,30 36,36 36,42 36,48 36,54 37,00 37:06 37:12 37,18
rile:S982310 #1-569 AcqslS-APX-1998 15,13,36 EI+ Voltag* SIX 70S Koiie>78
435.8169 r,4 BSUB(256,30,-3.0) PXD(7,5,3,0.05\,312.0,1.00\,T,T) ExpiNBBSUS
TSIAJfSLE LABS Text:TLIt45399 H23-RB-1-4 OKT. TIME •
1004 A1.0JX6
so:
eo:
401
20.
OJ
1.08E6
36,00 36,06 36:12 36,18 36,24 36:30 36,36 36:42 36:48 36:54 37:00 37:06 37:12 37:18
rile,S982310 fl-569 Acq,18-APR-1998 15,13,36 EI+ Voltage SIX 70S Jfoi«*:70
437.8140 T:4 BSOB(256,30;-3;0) PKD(7,5,3, 0. 051,280.0,1.00\,r,T) Exp-.HDBSVS
TRIANGLE LABS Tert:TLI#45399 M23-RB-1-4 XK7. TIME - 15:16
lOOSt Al.
ao:
eo:
40:
20:
36,00 36:06 36,12 36,18 36,24 36:30 36,36 36,42 36,48 36,54 37:00 37,06 37,12 37\18
rile,S982310 tl-569 Aotj,18-APX-1998 15,13:36 EI+ Voltage SIX 70S
430.9729 F,4 ExpttWBSVS
TRIANGLE LABS Text:TLIt45399 M23-XB-1-4 XK7. TIKE - 15:16
1001
so:
so:
40'.
20:
o:
36:08 36:14
36:53
37:08
.0.0X0
Tim*
O.OEO
Timt
_1.515
11. 3E5
.9.7X4
.6.5X4
.3.2X4
0.0X0
Time
1 . 6X5
1.3X5
9.5X4
6.3X4
3.2X4
0.0X0
36:00 36,06 36,12 36:18 36:24 36:30 36:36 36,42 36:48 36:54 37:00 37,06 37:12 37,18
.3.5X5
.2.8X5
.2.1X5
.1.4X5
.7.0X4
.0.0X0
Time
372
-------
1 Ue, si 823 Id H-S69 Acq,l8-APX-l998 IS, 13,36 EH- voltmge SIX 70S moime,4i
441.7428 Ti4 BSOB(256,30,-3.0) PKD(7, 5, 3,0. 051,164. 0,1.00\,r,T) ExptKDBSOS
TXIAHBLX LABS TextiTLIt45399 M23-XB-1-4 IK7. TIME - 15»15
1004 r2.4JM
901
801
701
601
501
40.
301
20.
10.
File
443.
TXIA1
100J
901
801
701
601
501
401
30.
20.
10.
File
430.
TXIA
1001
901
801
701
6ol
soj
40J
30j
20.
10-
0.
F±lt
513.
TXI1
1001
90.
80.
70.
60.
50.
40.
30
20
10
0
----•*- A Aw
3.2X4
1.9X4
1.7X4
.1.4X4
.1.2X4
.9.6X3
.7.2X3
.4.8X3
.2.4X3
0.0X0
35:00 37:00 38:00 39:00 40.00 41»00 42:00 Time
,3982310 tl-569 Acqtl8-APX-1998 15:13:35 EI+ Voltage SIX 70S Hoiaei41
7399 Tt4 BSUB(256,30,-3.0) PXD(7,5,3,0.05\,164.0,1.00\,T,T) ErptHDBSUS
HOLE LABS TexttTLIt45399 M23-XB-1-4 HKT. TIME - 15:15
-1.7X4
f* r -f "t r* r
, ..... A.
35:00 37:00 38:00 39:00 40:00 41:00 42:00
.5982310 tl-569 Acqtl8-APX-199S 15.13.35 EX+ Voltage SIX 70S
9729 Fi4 XxpiSDBSUS
OGLE LABS TerttTLIt45399 M23-XB-1-4 IJTJ: TIME - 15:15
"^^i^^^
' 35:00 ' ' 37:00 ' 38:00 39:00 40:00 41:00 42:00
>:5982310 *l-559 AcqilB-APS-1998 15:13:35 EI+ Voltage SIX 70S
6775 Tit EzptSDBSUS
\SSLE LABS Text:TLIt45399 M23-XB-1-4 IKT. TIME - 15:16
.36i3' , 37.J4 "I06 ^ 39,03
\*H^j^j^*ty(Ajk*dy^~*iSVii/i**^ir'^
36x 00 ' 37\00 38*00 39*00
.^J&X^^
40:00 41:00 42:00
J..6E4
.1.4X4
.1.2X4
.1.0E4
.8.7X3
.7.0X3
.5.2X3
.3.5X3
11.7X3
Time
-.3.6X5
.3.3X5
.2.9X5
.2.6X5
.2.2X5
.1.8X5
.1.5X5
.1.1X5
.7.3X4
.3.6X4
0.0X0
Time
-.3.8X3
.3.5X3
13.1X3
12.7X3
.2.3X3
.1.9X3
.1.5X3
.1.2X3
• -.7.7X2
'.3.8X2
'0.0X0
Time
-------
40i36 40's42 40:4t 40', 54 41tOO 41tOS
Fll»iS982310 #1-569 Acq,18-AfX-1998 15tl3i36 XI+ Voltag* SIX 70S Xoi»»:38
59.7348 r>4 BSUB(256,30,-3.0) m(7,5,3,0.05\,152.0,1.00\,r,T) ExptNDBSUS
TRIANGLE LABS T»xt:TLI«45399 M23-M3-1-4 UKT. TIMS " 15«Iff
2001
91-569 Acq,18-APS-1998 15sl3:Jl> SI* Volt»g» SIS JOS
57.7377 Fi4 BSUB(256r30, -3.0) PXD(7,5,3, 0.05%, 156.0,1.00\,T,T) XxpsHDBSOS
TRIANGLX LABS T+xt:TLH45399 M23-MB-1-4 OKT. TIMX - 15tl6
41112
so:
60.
40.
20.
A245.59
-r
T
-r
T
T
40,36 40', 42 40', 48 40:54 41:00 41:05
ril»iS982310 il-569 Aoqtl8-APX-1998 15:13:36 11+ Voltage SIR 70S Bo±*»:43
469.7779 T:4 BSUB(256f30,-3.0) PXD(7,5,3, 0.05\,172.0,1 .OQ\,T,T) ExptHDBSOS
TRIANGLE LABS T«xt:TLI*45399 M23-U-1-4 JWJ. HUE - 15tl6
lOOi, A1.55E6
'll': 12
40 36 40:42 - 40:48 40:54 41:00 41:06
Tile,S962310 tl-569 Acq:18-APX-1998 15>13:36 EI+ Voltage SIS 70S Koiae:41
471.7750 T:4 BSOB(256r30^-3:0) PXD(7,5,3,0.051,164.0,1.00\,f,T) ExpsODBSOS
TRIANGLE LABS TfXt:TLIt45399 H23-XB-1-4 INJ. TINE - 15s 16
ion AI.
41s 12
0.
40 36 40,42 40,48 40',54 41:00 41:06
ril»:S982310 tl-569 Acq:18-APX-1998 15,13,36 EH- Voltag* SIR 70S
430.9729 F:4 EipiNDBSUS
TRIANGLE LABS T*XtsTLIt45399 M23-XB-1-4 1X7. TIKE - 15,16
1004 , 40j41 40,51 _ 41:00
80.
60.
40.
20.
41:12
.2.7X2
.2.2X2
'.1.6X3
'.1.1X2
_5.5«
0.0X0
.1.7X5
'.1.3X5
.9.9X4
.6.6X4
.3.3X4
0.0X0
Tim*
-1.9X5
.1.5X5
.1.2X5
'.7.7X4
.3.9X4
40:36
40:42
40:4»
40:54
41:00
41:06
41s 12
3.5X5
2.8X5
2.1X5
1.4X5
.7.0X4
.0. 0X0
Tims
-------
Channel I 338,979£ Peak top
Height ,33 volts Span 299 ppi
Systet file naie
Dka file naie
Resolution
Grotpnutor
lonizatlon aode
Switching
• lasses 232.9825,
W65US
f):S982384
R 233
B 384
C 386
0 316
E 318
F 329
6 322
H 328
I 331
J 331
K 332
I 334
H 346
H 342
0 3S2
P 354
Q 356
R 358
2
Q*
VOL1NE
416.9768
6 368
T 379
U 376
V 418
Ref. nss 416,9768 Peak top
Height .98 volts Span 298 ppi
•'\
-------
CALIBRATION
DATA
THangfo Laboratories, Inc.
801 CapftotoOrftw P.O. Box 13485
Durham, NC 277134411 Hiamrch Trttn&t Ptrk, MC 277Q9-348Z
919-544-5729 - Fix 1919-544-5491
-------
Initial Calibration Summary for UF51058
Analysis Date : 01/05/98
Instrument : U
Analytes
Total MCDF
Total MCDD
Total DCDF
Total DCDD
Total TriCDF
Total TriCDD
1368-TCDF
2378-TCDF
TOTAL TCDF
1363-TCDD
1379-TCDD
2378-TCDD
TOTAL TCDD
12373-PeCDF
23473-PeCDF
•TOTAL PeCDF
12373-PeCDD
TOTAL PeCDD
123473-ExCDF
123678-HxCDF
234673-HxCDF
123789-HxCDF
TOTAL HxCDF
"123478-HxCDD
123673-HxCDD
123739-HxCDD
TOTAL HxCDD
1234678-HpCDF
1234789-HpCDF
TOTAL HpCDF
1234678-HpCDD
TOTAL HpCDD
OCDF
OCDD
Other Standards
37C1-TCDD
13C12-PeCDF 234
13C12-HxCDF 478
13C12-HxCDF 234
13C12-HxCDF 789
13C12-HXCDD 478
13C12-HpCDF 789
RF
0.000
0.000
0.000
0.000
0.000
0.000
.298
.240
.240
0.715
0.360
.240
.240
1.051
1.019
1.035
1.333
1.333
1.0C7
1.253
0.985
0.870
1.029
0.755
0.975
.941
.894
1
1,
1
1,
1
0,
0
1.410
1.095
1.253
0.995
0.995
1.377
1.108
SD
0.000
0.000
0.000
0.000
0.000
0.000
0.073
0.132
0.132
0.032
0.021
0.160
0.160
0.090
0.078
0.084
0.125
0.125
0.074
0.089
0.082
0.047
0.071
0.051
0.079
0.063
0.064
0.098
0.071
0.084
0.051
0.051
0.070
0.080
RF SD
1.001 0.056
0.966 0.010
0.825 0.042
0.902 0.043
0.695 0.042
0.732 0.024
0.802 0.016
%RSD
100%
100%
100%
100%
100%
100%
6%
11%
11%
4%
6%
13%
13%
9%
8%
8%
9%
9%
7%
7%
3%
5%
7%
7%
8%
7%
7%
7%
6%
7%
5%
5%
5%
7%
%RSD
6%
1%
5%
5%
6%
3%
2%
•£*«
RT
21:26
24:36
22:46
23:10
25:19
28:33
29:14
29:34
32:01
32:07
32:36
33:22
32:43
32:47
33:05
35:00
36:31
36:01
39:47
39:35
RT
25:19
29:14
32:01
32:35
33:21
32:42
36:30
RT/LO
4:35
5:18
11:35
12:18
15:35
17:18
23:35
24:18
24:32
25:34
23:06
28:47
30:59
32:00
35:34
35:34
RT/LO
23:18
26:32
32:59
RT/HI I
18:35
19:18
19:35
20:18
22:35
23:18
30:35
31:18
32:32
33:34
36:06
36:47
38:59
40:00
43:34
43:34
RT/HI
27:18
30:32
38:59
k «•
latiol Ratio2
0.745
0.743
0.744
0.776
0.786
0.737
0.731
1.525
1.53Q
1.523
1.530
1.530
1.233
1.245
1.262
1.253
1.262
1.257
1.211
1.234
1.232
1.060
1.049
1.055
1.023
1.028
0.891
0.836
Ratiol Ratio2
1.498
0.509
0.508
0.504
1.214
0.431
N
0
0
0
0
0
0
6
6
6
6
6
6
6
5
6
5
6
6
6
6
6
6
6
6
6
6
6
6
6
6
6
6
6
6
N
6
6
6
6
6
6
6
Page
Triangle Laboratories, IncjS Analytieal Service* Division
801 Capitola Drive • Durham, North Caroina 27713
Phone: (919) 544-5729 • Fax (919) 544-5491
Printed: 15:16
-------
Internal Standards
13C12-2378-TCDF
13C12-2378-TCDD
13C12-PeCDF 123
13C12-PeCDD 123
13C12-HxCDF 678
13C12-HxCDD 678
13C12-HpCDF 678
13C12-HpCDD 678
13C12-OCDD
RF
1.
1.
1.
0.
1.
0,
0
Q
0
467
118
142
,590
.346
.995
.822
.726
.545
0
0
0
0
0
0
0
0
0
SD
.053
.049
.075
.045
.038
.017
.013
.011
.038
%RSD
4%
4%
7%
8%
3%
2%
2%
2%
7%
BT
24:35
25:18
28:32
29:34
32:06
32:47
34:59
36:00
39:34
KT/LQ
23:35
23:18
24:32
25:34
28:06
31:47
32:59
35:00
37:34
RT/HI
25:35
27:18
32:32
33:34
36:06
33:47
38:59
37:00
41:34
Ratio 1
0.7S5
0.807
1.478
1.S06
0.506
1.216
0.434
1.018
0.861
Ratio2
Recovery Standards RF SD %RSD
13C12-1234-TCDD 1.000 0.000 0%
13C12-HxCDD 789 1.000 0.000 0%
*** End of Report **"
RT
25:08
33:05
RT/LO RT/HI
Ratio1
0.812
1.210
Ratio2
N
6
6
6
6
6
6
6
6
6
6
6
Page
Triangle laboratories, bio« Analytical Services DMston
901 Capftote Drive •Durtam. North Cwofam 27713
Phone: (919) 544-5729 • Fee (919) 544-5491
Printed: 15:16 01/1
o i •
-------
Continuing Calibration Cor O980771
Init Calibration
ICal Date
Analyte Sunnary
Name
Total MCDF
Total MCOD
Total DCDF
Total DCDD
Total TriCDF
Total TriCDD
1368-TCDF
2378-TCDF
TOTAL TCDF
1368-TCDD
1379-TCDD
2378-TCDD
TOTAL TCDD
12378-PeCDF
23478-PeCDF
TOTAL PeCDF
12378-PeCDD
TOTAL PeCDD
123478-HxCDF
• DL
' M
. : XJP51058
• 01/05/98
Instrument
Std.Conc
9
«•
10.00
ICal Delta
RF Ratio RT RT Rel. RT RP RF %D
1*2 Lo/High
0.000 3:22 0.000 0.000 100.0%
17:22
0.000 4:08 0.000 0.000 100.0%
18:08
0.000 10:22 0.000 0.000 100.0%
18:22
0.000 11:08 0.000 0.000 100.0%
0.000
0.000
1.285
1.227
1.227
0.702
0.321
1.125
1.125
1.081
1.056
1.069
1.250
1.250
1.210
0.76
0.77
0.76
0.79
0.78
0.78
0.78
1.51
1.49
1.50
1.61
1.61
1.26
19:
14:
21:
16:
22:
19:
25:
21:
25:
25
29
26
29
30
08
22
22
08
08
43 19:55 0.8524
22
23:23 1.0007
12 21:24 0.8867
:20
21:50 0.9047
24:09 1.0007
:16 27:34 1.0006
:26
28:18 1.0272
:35 28:39 1.0000
:17
:00 31:10 0.9968
0.000
0.000
1.298
1.240
1.240
0.715
0.360
1.240
1.240
1.051
1.019
1.035
1.333
1.333
1.007
0.000 100.0%
0.000 100.
-0.013
-0.013
-0.013
-0.013
-0.039
-0.115
-0.115
0.030
0.037
0.034
-0.083
-0.083
0.203
-1.
-1.
-1.
-1.
-10.
-9.
0%
0%
1%
1%
9%
3%
3%
-9.3%
2.9%
3.6%
3
-6
-6
20
.2%
.2%
.2%
.2%
32:44
123678-HxCDF
234678-HxCDF
123789-HXCDF
1.267
1.053
1.031
1.24
1.28
1.30
31:17 1.0005
31:46 1.0160
32:30 1.0394
1.253
0.985
0.870
0.014
0.068
0.161
1
6
18
.1%
.9%
.5%
Page 1
Triangle Laboratories, Inc.® Analytical Services Division
801 Capttola Drive • Durham, North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 14:20 04/15/9
-------
uace: y«/ia/»o
TK.LAMUUB UAMUKATUtCLIUi U* KTP, IMt .
Continuing Calibration tor 0980771
TOTAL HxCDF
123 47 8 -HxCDD
123678-HXCDD
123789-HxCDD
TOTAL HxCDD
1234678-HpCDF
12347 89-HpCDF
TOTAL HpCDF
1234678-HpCDD
TOTAL HpCDD
OCDF
OCDD
1.140 1.27
0.878 1.21
0.916 1.22
0.910 1.22
0.901 1.21
1.377 1.06
1.115 1.06
1.246 1.06
1.008 1.02
1.008 1.02
1.279 0.91
1.001 0.87
30:31 31:53 0.9979
32:24
31:58 1.0005
32:16 1.0099
33:54 34:05 1.0005
35:41
35:31 1.0426
34:10 35:04 1.0005
35:13
34:23 38:34 1.0048
42:23
34:23 38:24 1.0004
42:23
Other Standard Sumnary
Name
37C1-TCDD
13C12-PeCDF 234
13C12 -HxCDF 478
13C12-HXCDF 234
13C12-HXCDF 789
13C12 -HxCDD 478
13C12-HpCDF 789
RF Ratio
142
0.972
0.932 1.47
1.005 0.51
0.977 0.50
0.834 0.49
0.939 1.20
0.366 0.42
RT RT Rel. RT
Lo/High
22:08 24:09 1.0007
26:08
23:33 28:17 1.0266
31:33
31:10 0.9968
31:46 1.0160
32:30 1.0394
31:53 0.9979
32:04 35:31 1.0426
38:04
Internal Standard Summary
Name
13C12-2378-TCDF
13C12-2378-TCDD
13C12-PeCDF 123
RF Ratio
1&2
1.484 0.76
1.121 0.81
1.085 1.49
RT RT Rel. RT
Lo/High
22:22 23:22 1.0000
24:22
22:08 24:08 1.0000
26:08
23:33 27:33 1.0000
31:33
Page 2
1.029 0.111 10.8%
0.765 0.113 14.8%
0.976 -0.060 -6.1%
0.941 -0.031 -3.3%
0.894 0.007 0.8%
1.410 -0.033 -2.3%
1.096 0.019 1.7%
1.253 -0.007 -0.6%
0.995 0.013 1.3%
0.995 0.013 1.3%
1.377 -0.098 -7.1%
1.108 -0.107 -9.6%
ICal Delta
RF RF %D
1.001 -0.029 -2.9%
0.966 -0.034 -3.5%
0.825 0.180 21.9%
0.902 0.075 8.3%
0.695 0.139 20.0%
0.732 0.207 28.3%
0.802 0.064 8.0%
ICal Delta
RF RF %D
1.467 0.017 1.2%
1.118 0.003 0.2%
1.142 -0.057 -5.0%
Triangle Laboratories, Inc.® Analytical Services Division
801 Cap'rtola Drive • Durham, North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 14:20 04H»98.
*f(.
-------
« Continuing Calibration for 0980771
13C12-P«CDD 123 0.607 1.46 24:39 28:39 1.0000 0.590 0.017 2.8%
32:39
13C12-HXCDP 678 1.289 0.51 27:16 31:16 1.0000 1.346 -0.057 -4.3%
35:16
13C12-BxCDO 678 1.043 1.23 30:57 31:57 1.0000 0.995 0.048 4.8%
32:57
13C12-HpCDP 678 0.879 0.43 32:04 34:04 1.0000 0.822 0.057 6.9%
38:04
13C12-HpCDD 678 0.741 1.06 34:03 35:03 1.0000 0.726 0.015 2.1%
36:03
13C12-OCDD 0.569 0.88 38:12 38:23 1.0000 0.545 0.024 4.3%
38:32
Recovery Standard Suratary ICal Delta
Name RF Ratio RT RT R*l. RT RF RF %D
1&2 Lo/High
13C12-1234-TCDD 1.000 0.82 23:56 0.9917 1.000 0.000 0.0%
13C12-HXCDD 789 1.000 1.20 32:15 1.0094 1.000 0.000 0.0%
QC Front End Check: 1.S693
Page
Triangle Laboratories, Inc.® Analytical Sarvlcas DrvUlon
801 Capitals Drive • Durham, North Carolina 27713 Printed: 14:20 04/15/
Phone: (919) 544-5729 • Fax: (919) 544-5491
-------
APPENDIX C
CALCULATIONS
-------
-------
Summary of Stack Gas Parameters and Test Results
Air Emissions Screening Test
Chemical Lime Company - Alabaster, Alabama
US EPA Test Method 23 - PCDDs / PCDFs
Kiln # 1 Scrubber Inlet
Page 1 of 6
RUN NUMBER
RUN DATE
RUN TIME
M23-I-3
3/26/98
1300-1621
Y
AH
Pbar
•"static
Ts
C02
02
N2
C
Ap
0
Dn
'P
1/2
'm(std)
V
mfstd)
P,
1-Bws
Md
M.
V.
A
Qa
Q.
Q»(cnim)
I .
MEASURED DATA
Meter Box Correction Factor 1.021
Avg Meter Orifice Pressure, in. H20 0.93
Barometric Pressure, inches Hg 29.50
Sample Volume, ft3 91.987
Average Meter Temperature, °F 101.8
Stack Static Pressure, inches H20 -4.60
Average Stack Temperature, °F 775
Condensate Collected, ml 320.5
Carbon Dioxide content, % by volume 20.0
Oxygen content, % by volume 10.0
Nitrogen content, % by volume 70.0
Pitot Tube Coefficient 0.84
Average Square Root Ap, (in. H20)1C 0.6865
Sample Run Duration, minutes 180
Nozzle Diameter, inches 0.250
CALCULATED DATA
Nozzle Area, ft2 0.00034
Standard Meter Volume, dscf 87.202
Standard Meter Volume, dscm 2.469
Stack Pressure, inches Hg 29.16
Moisture, % by volume 14.7
Standard Water Vapor Volume, ft3 15.086
Dry Mole Fraction 0.853
Molecular Weight (d.b.), lb/lb»mole 31.60
Molecular Weight (w.b.), Ib/lb-mole 29.59
Stack Gas Velocity, ft/s 59.0
Stack Area, ft2 25.00
Stack Gas Volumetric flow, acfm 88,472
Stack Gas Volumetric flow, dscfm 31,410
Stack Gas Volumetric flow, dscmm 889
Isokinetic Sampling Ratio. % 113.1
E:\r012.002\Alabaste.r\Data\M23alab.xls, Sum I-3
-------
Summary of Stack Gas Parameters and Test Results
Chemical Lime Company - Alabaster, Alabama
US EPA Test Method 23 - PCDDs / PCDFs
Kiln # 1 Scrubber Inlet
Page 2 of 6
RUN NUMBER
RUN DATE
RUN TIME
M23-I-3
3/26/98
1300-1621
EMISSIONS DATA
DIOXINS:
2378 TCDD
ng Catch, ng (0.003)
ng/dscm Concentration, ng/dscm, as measured (0.00121)
ug/hr Emission Rate, ug/hr (0.0648)
Total TCDD
ng Catch, ng 0.01
ng/dscm Concentration, ng/dscm, as measured 0.00405
ug/hr Emission Rate, ug/hr 0.216
12378 PeCDD
ng Catch, ng (0.004)
ng/dscm Concentration, ng/dscm, as measured (0.00162)
ug/hr Emission Rate, ug/nr (0.0864)
Total PeCDD
ng Catch, ng ' (0.004)
ng/dscm Concentration, ng/dscm, as measured (0.00162)
ug/hr Emission Rate, ug/hr (0.0864)
123478 HxCDD
ng Catch, ng (0.007)
ng/dscm Concentration, ng/dscm, as measured (0.00283)
ug/hr Emission Rate, ug/hr (0.151)
123678 HxCDD
ng Catch, ng (0.007)
ng/dscm Concentration, ng/dscm, as measured (0.00283)
ug/hr Emission Rate, ug/hr (0.151)
() Not Detected. Value shown is the detection limit and is included hi totals.
{} Estimated Maximum Possible Concentration. EMPC values are included in totals.
E:\r012.002\Alabaste.r\Data\M23alab.xls, Sum 1-3
-------
Summary of Stack Gas Parameters and Test Results
Chemical Lime Company - Alabaster, Alabama
US EPA Test Method 23 - PCDDs / PCDFs
Kiln # 1 Scrubber Inlet
Page 3 of 6
RUN NUMBER
RUN DATE
RUN TIME
M23-I-3
3/26/98
1300-1621
ng
ng/dscm
ug/hr
ng
ng/dscm
ug/hr
ng
ng/dscm
ug/hr
ng
ng/dscm
ug/hr
ng
ng/dscm
ug/hr
ng
ng/dscm
ug/hr
EMISSIONS DATA -Continued
DIOXINS - Continued
1 23789 HxCDD
Catch, ng
Concentration, ng/dscm, as measured
Emission Rate, ug/hr
Total HxCDD
Catch, ng
Concentration, ng/dscm, as measured
Emission Rate, ug/hr
1234678
Catch, ng
Concentration, ng/dscm, as measured
Emission Rate, ug/hr
Total HpCDD
Catch, ng
Concentration, ng/dscm, as measured
Emission Rate, ug/hr
OCDD
Catch, ng
Concentration, ng/dscm, as measured
Emission Rate, ug/hr
Total PCDD
Catch, ng
Concentration, ng/dscm, as measured
Emission Rate, ug/hr
(0.007)
(0.00283)
(0.151)
(0.007)
(0.00283)
(0.151)
(0.01)
(0.00405)
(0.216)
(0.01)
(0.00405)
(0.216)
{0.03}
{0.0121}
{0.648}
(0.061)
(0.0247)
(1 .32)
() Not Detected. Value shown is the detection limit and is included in totals.
{} Estimated Maximum Possible Concentration. EMPC values are included in totals.
E:\r012.002\Alabaste.r\Data\M23alab.xls, Sum I-3
-------
Summary of Stack Gas Parameters and Test Results
Chemical Lime Company - Alabaster, Alabama
US EPA Test Method 23 - PCDDs / PCDFs
Kiln # 1 Scrubber Inlet
Page 4 of 6
RUN NUMBER
RUN DATE
RUN TIME
M23-I-3
3/26/98
1300-1621
EMISSIONS DATA - Continued
FURANS
2378 TCDF
ng Catch, ng {0.007}
ng/dscm Concentration, ng/dscm, as measured {0.00283}
ug/hr Emission Rate, ug/hr {0.151}
Total TCDF
ng Catch, ng 0.11
ng/dscm Concentration, ng/dscm, as measured 0.0445
ug/hr Emission Rate, ug/hr 2.38
12378 PeCDF
ng Catch, ng (0.003)
ng/dscm Concentration, ng/dscm, as measured (0.00121)
ug/hr Emission Rate, ug/hr (0.0648)
23478 PeCDF
ng Catch, ng (0.003)
ng/dscm Concentration, ng/dscm, as measured (0.00121)
ug/hr Emission Rate, ug/hr (0.0648)
Total PeCDF
ng Catch, ng 0.02
ng/dscm Concentration, ng/dscm, as measured 0.00810
ug/hr Emission Rate, ug/hr 0.432
123478 HxCDF
ng Catch, ng {0.007}
ng/dscm Concentration, ng/dscm, as measured {0.00283}
ug/hr Emission Rate, ug/hr {0.151}
() Not Detected. Value shown is the detection limit and is included in totals.
{} Estimated Maximum Possible Concentration. EMPC values are included in totals.
E:\rf)12.002\Alabaste.r\Data\M23alab.xls, Sum I-3
-------
Summary of Stack Gas Parameters and Test Results
Chemical Lime Company - Alabaster, Alabama
US EPA Test Method 23 - PCDDs / PCDFs
Kiln # 1 Scrubber Inlet
Page 5 of 6
RUN NUMBER
RUN DATE
RUN TIME
M23-I-3
3/26/98
1300-1621
EMISSIONS DATA - Continued
Furans - Continued
123678 HxCDF
ng Catch, ng {0.04}
ng/dscm Concentration, ng/dscm, as measured {0.0162}
ug/hr Emission Rate, ug/hr {0.864}
234678 HxCDF
ng Catch, ng (0.004)
ng/dscm Concentration, ng/dscm, as measured (0.00162)
pg/hr Emission Rate, ug/hr (0.0864)
123789 HxCDF
ng Catch, ng (0.005)
ng/dscm Concentration, ng/dscm, as measured (0.00202)
ug/hr Emission Rate, ug/hr (0.108)
Total HxCDF
ng Catch, ng 0.01
ng/dscm Concentration, ng/dscm, as measured 0.00405
ug/hr Emission Rate, ug/hr 0.216
1234678 HpCDF
ng Catch, ng 0.009
ng/dscm Concentration, ng/dscm, as measured 0.00364
ug/hr Emission Rate, ug/hr 0.195
1234789 HpCDF
ng Catch, ng (0.008)
ng/dscm Concentration, ng/dscm, as measured (0.00324)
ug/hr Emission Rate, pg/hr (0.173)
() Not Detected. Value shown is the detection limit and is included in totals.
{} Estimated Maximum Possible Concentration. EMPC values are included in totals.
E:\r012.002\Alabaste.r\Data\M23alabjds. Sum 1-3
-------
Summary of Stack Gas Parameters and Test Results
Chemical Lime Company - Alabaster, Alabama
US EPA Test Method 23 - PCDDs / PCDFs
Kiln # 1 Scrubber Inlet
Page 6 of 6
RUN NUMBER
RUN DATE
RUN TIME
M23-I-3
3/26/98
1300-1621
EMISSIONS DATA - Continued
Furans - Continued
Total HoCDF
ng Catch, ng 0.009
ng/dscm Concentration, ng/dscm, as measured 0.00364
ug/hr Emission Rate, ug/hr 0.195
OCDF
ng Catch, ng (0.02)
ng/dscm Concentration, ng/dscm, as measured (0.00810)
ug/hr Emission Rate, ug/hr (0.432)
Total PCDF
ng Catch, ng (0.169)
ng/dscm Concentration, ng/dscm, as measured (0.0684)
ug/hr Emission Rate, ug/hr (3.65)
Total PCDD + PCDF
ng Catch, ng (0.230)
ng/dscm Concentration, ng/dscm, as measured (0.0931)
ug/hr Emission Rate, ug/hr (4.97)
() Not Detected. Value shown is the detection limit and is included in totals.
{} Estimated Maximum Possible Concentration. EMPC values are included in totals.
E:\r012.002\Alabaste.r\Data\M23alab.xls, Sum I-3
-------
Summary of Stack Gas Parameters and Test Results
Air Emissions Screening Test
Chemical Lime Company - Alabaster, Alabama
US EPA Test Method 23 - PCDDs / PCDFs
Kiln # 1 Scrubber Stack
Page 1 of 6
RUN NUMBER
RUN DATE
RUN TIME
M23-O-3
3/26/98
1300-1632
COS(lfl) * Ap
0
Dr
An
1/2
MEASURED DATA
y Meter Box Correction Factor 1.000
AH Avg Meter Orifice Pressure, in. H2O 1.84
Pta, Barometric Pressure, inches Hg 29.50
Vm Sample Volume, ft3 131.716
Tm Average Meter Temperature, *F 88.4
P«tatic Stack Static Pressure, inches H2O -0.41
T, Average Stack Temperature, °F 137
Vfc Condensate Collected, ml 712.7
CO2 Carbon Dioxide content, % by volume 20.0
O2 Oxygen content, % by volume 10.0
N2 Nitrogen content, % by volume 70.0
Cp Pilot Tube Coefficient 0.84
Average Square Root Ap, (in. H2O)1'1
Ap1Q In Flow Direction 0.7494
In Axial Direction 0.6481
Sample Run Duration, minutes 187.8
Nozzle Diameter, inches 0.250
CALCULATED DATA
Nozzle Area, ft2 0.00034
Standard Meter Volume, dscf 125.554
Standard Meter Volume, dscm 3.555
P, Stack Pressure, inches Hg 29.47
BW, Moisture, % by volume 21.1
Bw«ut) Moisture (at saturation), % by volume 18.6 (used
VW.M Standard Water Vapor Volume, ft3 33.547
1-B*. Dry Mole Fraction 0.814
Md Molecular Weight (d.b.), Ib/lb-mole 31.60
M. Molecular Weight (w.b.). Ib/lb-mole 29.07
Stack Gas Velocity, ft/s
V, In Flow Direction 44.93
Vu In Axial Direction 38.86
A Stack Area, ft2 18.35
Qa Stack Gas Volumetric flow, acfm 42,775
Q, Stack Gas Volumetric flow, dscfm 30,316
Q«cnm) Stack Gas Volumetric flow, dscmm 858
I Isokinetic Sampling Ratio. % 102.7
E:\r012.002\Alabaste.rtData\M23alabals, Sum O-3
-------
Summary of Stack Gas Parameters and Test Results
Chemical Lime Company - Alabaster, Alabama
US EPA Test Method 23 - PCDDs / PCDFs
Kiln #1 Scrubber Stack
Page 2 of 6
RUN NUMBER
RUN DATE
RUN TIME
M23-O-3
3/26/98
1300-1632
ng
ng/dscm
pg/hr
EMISSIONS DATA
DIOXINS:
2378 TCDD
Catch, ng
Concentration, ng/dscm, as measured
Emission Rate, pg/hr
Total TCDD
ng Catch, ng
ng/dscm Concentration, ng/dscm, as measured
pg/hr Emission Rate, pg/hr
12378 PeCDD
ng Catch, ng
ng/dscm Concentration, ng/dscm, as measured
ug/hr Emission Rate, pg/hr
Total PeCDD
ng Catch, ng
ng/dscm Concentration, ng/dscm, as measured
pg/hr Emission Rate, pg/hr
123478 HxCDD
ng Catch, ng
ng/dscm Concentration, ng/dscm, as measured
pg/hr Emission Rate, ug/hr
123678 HxCDD
ng Catch, ng
ng/dscm Concentration, ng/dscm, as measured
pg/hr Emission Rate, pg/hr
(0.006)
(0.00169)
(0.0869)
(0.006)
(0.00169)
(0.0869)
(0.009)
(0.00253)
(0.130)
(0.009)
(0.00253)
(0.130)
(0.01)
(0.00281)
(0.145)
(0.01)
(0.00281)
(0.145)
() Not Detected. Value shown is the detection limit and is included in totals.
{} Estimated Maximum Possible Concentration. EMPC values are included in totals.
E:\r012.002\Alabaste.r\Data\M23alabJds, Sum O-3
-------
Summary of Stack Gas Parameters and Test Results
Chemical Lime Company - Alabaster, Alabama
US EPA Test Method 23 - PCDDs / PCDFs
Kiln # 1 Scrubber Stack
Page 3 of 6
RUN NUMBER
RUN DATE
RUN TIME
M23-O-3
3/26/98
1300-1632
ng
ng/dscm'
pg/hr
EMISSIONS DATA-Continued
DIOXINS - Continued
123789 HxCDD
Catch, ng
Concentration, ng/dscm, as measured
Emission Rate, pg/hr
Total HxCDD
ng Catch, ng
ng/dscm Concentration, ng/dscm, as measured
pg/hr Emission Rate, pg/hr
1234678 HoCDD
ng Catch, ng
ng/dscm Concentration, ng/dscm, as measured
pg/hr Emission Rate, pg/hr
Total HpCDD
ng Catch, ng
ng/dscm Concentration, ng/dscm, as measured
pg/hr Emission Rate, pg/hr
OCDD
ng Catch, ng
ng/dscm Concentration, ng/dscm, as measured
pg/hr Emission Rate, pg/hr
Total PCDD
ng Catch, ng
ng/dscm Concentration, ng/dscm, as measured
pg/hr Emission Rate, pg/hr
(0.009)
(0.00253)
(0.130)
(0.01)
(0.00281)
(0.145)
(0.01)
(0.00281)
(0.145)
(0.01)
(0.00281)
(0.145)
(0.02)
(0.00563)
(0.290)
(0.055)
(0.0155)
(0.797)
() Not Detected. Value shown is the detection limit and is included in totals.
{} Estimated Maximum Possible Concentration. EMPC values are included in totals.
E:\r012.002Wabaste.r\Data\M23alabjds, Sum O-3
-------
Summary of Stack Gas Parameters and Test Results
Chemical Lime Company - Alabaster, Alabama
US EPA Test Method 23 - PCDDs / PCDFs
Kiln #1 Scrubber Stack
Page 4 of 6
RUN NUMBER
RUN DATE
RUN TIME
M23-O-3
3/26/98
1300-1632
EMISSIONS DATA - Continued
FURANS
2378 TCDF
ng Catch, ng (0.007)
ng/dscm Concentration, ng/dscm, as measured (0.00197)
pg/hr Emission Rate, pg/hr (0.101)
Total TCDF
ng Catch, ng {0.007}
ng/dscm Concentration, ng/dscm, as measured {0.00197}
pg/hr Emission Rate, ug/hr {0.101}
12378PeCDF
ng Catch, ng (0.006)
ng/dscm Concentration, ng/dscm, as measured (0.00169)
pg/hr Emission Rate, ug/hr (0.0869)
23478 PeCDF
ng Catch, ng (0.006)
ng/dscm Concentration, ng/dscm, as measured (0.00169)
pg/hr Emission Rate, pg/hr (0.0869)
Total PeCDF
ng Catch, ng (0.006)
ng/dscm Concentration, ng/dscm, as measured (0.00169)
pg/hr Emission Rate, pg/hr (0.0869)
123478 HxCDF
ng Catch, ng (0.006)
ng/dscm Concentration, ng/dscm, as measured (0.00169)
pg/hr Emission Rate, pg/hr (0.0869)
() Not Detected. Value shown is the detection limit and Is Induded in totals.
{} Estimated Maximum Possible Concentration. EMPC values are included in totals.
E:\r012.002\Alabaste.r\Data\M23alabJds, Sum O-3
-------
Summary of Stack Gas Parameters and Test Results
Chemical Lime Company - Alabaster, Alabama
US EPA Test Method 23 - PCDDs / PCDFs
Kiln # 1 Scrubber Stack
Page 5 of 6
RUN NUMBER
RUN DATE
RUN TIME
M23-O-3
3/26/98
1300-1632
EMISSIONS DATA - Continued
Furans - Continued
123678 HxCDF
ng Catch, ng (0.006)
ng/dscm Concentration, ng/dscm, as measured (0.00169)
pg/hr Emission Rate, pg/hr (0.0869)
234678 HxCDF
ng Catch, ng (0.007)
ng/dscm Concentration, ng/dscm, as measured (0.00197)
ug/hr Emission Rate, ug/hr (0.101)
123789 HxCDF
ng Catch, ng (0.008)
ng/dscm Concentration, ng/dscm, as measured (0.00225)
pg/hr Emission Rate, ug/hr (0.116)
Total HxCDF
ng Catch, ng (0.007)
ng/dscm Concentration, ng/dscm, as measured (0.00197)
pg/hr Emission Rate, ug/hr (0.101)
1234678 HpCDF
ng Catch, ng (0.01)
ng/dscm Concentration, ng/dscm, as measured (0.00281)
pg/hr Emission Rate, pg/hr (0.145)
1234789 HpCDF
ng Catch, ng (0.01)
ng/dscm Concentration, ng/dscm, as measured (0.00281)
pg/hr Emission Rate, pg/hr (0.145)
() Not Detected. Value shown is the detection limn and is included in totals.
{} Estimated Maximum Possible Concentration. EMPC values are inducted in totals.
E:\r012.002\Alabaste.r\Data\M23alabjds, Sum O-3
-------
Summary of Stack Gas Parameters and Test Results
Chemical Lime Company - Alabaster, Alabama
US EPA Test Method 23 - PCDDs / PCDFs.
Kiln #1 Scrubber Stack
Page 6 of 6
RUN NUMBER
RUN DATE
RUN TIME
M23-O-3
3/26/98
1300-1632
EMISSIONS DATA - Continued
Furans - Continued
Total HoCDF
ng Catch, ng (0.01)
ng/dscm Concentration, ng/dscm, as measured (0.00281)
ug/hr Emission Rate, ug/hr (0.145)
OCDF
ng Catch, ng (0.01)
ng/dscm Concentration, ng/dscm, as measured (0.00281)
ug/hr Emission Rate, ug/hr (0.145)
Total PCDF
ng Catch, ng (0.040)
ng/dscm Concentration, ng/dscm, as measured (0.0113)
ug/hr Emission Rate, ug/hr (0.579)
Total PCDD + PCDF
ng Catch, ng (0.0950)
ng/dscm Concentration, ng/dscm, as measured (0.0267)
pg/hr Emission Rate, pg/hr (1.38)
() Not Detected. Value shown is the detection limit and is included in totals.
{} Estimated Maximum Possible Concentration. EMPC values are included in totals.
E:\r012.002\Alabaste.r\Data\M23alabjds, Sum O-3
-------
Summary of Stack Gas Parameters and Test Results
Air Emissions Screening Test
Chemical Lime Company - Alabaster, Alabama
US EPA Test Method 26A - HCI
Kiln No. 1 Scrubber Inlet
Page 1 of 2
Pstaflc
y
Pbar
vm
Ap1/2
AH
Tm
Ts
V|c
CO2
02
N2
Cp
0
Dn
An
Vm(std)
Vm(std)
Qm
PS
BWS
i-Sl
Md
Ms
Vs
A
Qa
Qs
Qs
I
RUN NUMBER
RUN DATE
RUN TIME
MEASURED DATA
Stack Static Pressure, inches H2O
Meter Box Correction Factor
Barometric Pressure, inches Hg
Sample Volume, ft3
Average Square Root Ap, (in. H2O)1/2
Avg Meter Orifice Pressure, in. H2O
Average Meter Temperature, *F
Average Stack Temperature, °F
Condensate Collected, ml
Carbon Dioxide content, % by volume
Oxygen content, % by volume
Nitrogen content, % by volume
Pilot Tube Coefficient
Sample Run Duration, minutes
Nozzle Diameter, inches
CALCULATED DATA
Nozzle Area, ft2
Standard Meter Volume, ft3
Standard Meter Volume, m3
Average Sampling Rate, dscfm
Stack Pressure, inches Hg
Moisture, % by volume
Standard Water Vapor Volume, ft3
Dry Mole Fraction
Molecular Weight (d.b.), lb/lb«mole
Molecular Weight (w.b.), Ib/lb-mole
Stack Gas Velocity, ft/s
Stack Area, ft2
Stack Gas Volumetric flow, acfm
Stack Gas Volumetric flow, dscfm
Stack Gas Volumetric flow, dscmm
Isokinetic Sampling Ratio, %
I-M26A-1
3/27/98
0907-1016
-4.10
1.021
29.50
33.216
0.6820
1.12
87.4
784
127.6
20.00
10.00
70.0
0.84
60
0.275
0.000412
32.329
0.915
0.539
29.20
15.7
6.006
0.843
31.60
29.47
58.9
25.00
82,606
28,833
816
105.9
I-M26A-2
3/27/98
1140-1255
-3.70
1.021
29.50
30.471
0.6093
0.90
95.7
781
131.5
20.00
10.0
70.0
0.84
60
0.275
0.000412
29.201
0.827
0.487
29.23
17.5
6.190
0.825
31.60
29.22
52.7
25.00
79,121
27,113
768
108.8
I-M26A-3
3/27/98
1422-1536
-3.70
1.021
29.50
39.582
0.6129
1.57
101
775
151.3
20.00
10.00
70.0
0.84
60
0.312
0.000531
37.602
1.065
0.627
29.23
15.9
7.122
0.841
31.60
29.43
52.7
25.00
79,098
27,765
786
106.3
Average
-3.83
1.021
29.50
34.423
0.6347
1.19
94.8
780
136.8
20.0
10.0
70.0
0.84
60
0.287
0.000452
33.044
0.936
0.551
29.22
16.4
6.439
0.836
31.60
29.37
54.8
25.00
80,275
27,904
790
107.0
E*012.002\Alabatte.rtData\M26a-injd» - Summttf
-------
Summary of Stack Gas Parameters and Test Results
Air Emissions Screening Test
Chemical Lime Company - Alabaster, Alabama
US EPA Test Method 26A - HCI
Kiln No. 1 Scrubber Inlet
Page 2 of 2
Fw,
Cppmvd
EHC.
Fw,
^ppmvd
EC.
Fw,
Cppmvd
ENH4
Fw,
Cpprnvd
EA,
Fw,
r+
^•*ppnwd
EC.
Fw,
Cppmvd
EMg
Fw,
Cppmvd
EK
Fw,
Cppmvd
EN.
RUN NUMBER
RUN DATE
RUN TIME
EMISSIONS DATA
Chlorides as HCI
Target Catch, mg
Formula Weight, Ib/lb-mol
Concentration, ppm by volume
Emission Rate, Ib/hr
Chlorides as Cl
Target Catch, mg
Formula Weight, Ib/lb-mol
Concentration, ppm by volume
Emission Rate, Ib/hr
Ammonia as NH
Target Catch, mg
Formula Weight, Ib/lb-mol
Concentration, ppm by volume
Emission Rate, Ib/hr
Aluminum. Al
Target Catch, ug
Formula Weight, Ib/lb-mol
Concentration, ppm by volume
Emission Rate, Ib/hr
Calcium. Ca
Target Catch, ug
Formula Weight, Ib/lb-mol
Concentration, ppm by volume
Emission Rate, Ib/hr
Magnesium. Ma
Target Catch, ug
Formula Weight, Ib/lb-mol
Concentration, ppm by volume
Emission Rate, Ib/hr
Potassium. K
Target Catch, ug
Formula Weight, Ib/lb-mol
Concentration, ppm by volume
Emission Rate, Ib/hr
Sodium. Na
Target Catch, ug
Formula Weight, Ib/lb-mol
Concentration, ppm by volume
Emission Rate, Ib/hr
I4M26A-1 I-M26A-2 I-M26A-3
3/27/98 3/27/98 3/27/98
0907-1016 1140-1255 1422-1536
11.99
36.47
8.63
1.41
11.65
35.45
8.63
1.37
0.43
18.04
0.626
0.0507
#N/A
26.98
#N/A
#N/A
#N/A
40.08
#N/A
#N/A
#N/A
24.31
#N/A
#N/A
#N/A
39.10
#N/A
#N/A
#N/A
22.99
#N/A
#N/A
10.15
36.47
8.10
1.25
9.87
35.45
8.10
1.21
0.57
18.04
0.919
0.0700
(20.0)
26.98
(0.0216)
(0.00246)
150.0
40.08
0.109
0.0184
30.10
24.31
0.0360
0.00370
8.87
39.10
0.00660
0.00109
151.0
22.99
0.191
0.0185
-
20.51
36.47
12.7
2.00
19.94
35.45
12.7
1.95
0.65
18.04
0.814
0.0635
#N/A
26.98
#N/A
#N/A
#N/A
40.08
#N/A
#N/A
#N/A
24.31
#N/A
#N/A
#N/A
39.10
#N/A
#N/A
#N/A
22.99
#N/A
#N/A
Average
14.22
36.47
9.81
1.55
13.82
35.45
9.81
1.51
0.55
18.04
0.786
0.0614
(20.0)
26.98
(0.0216)
(0.00246)
150.0
40.08
0.109
0.0184
#N/A
24.31
0.0360
0.00370
8.87
39.10
0.00660
0.00109
151.0
22.99
0.191
0.0185
() - Not Detected
E:W12.002\Atab«*t».i\D*»\M26Hn.xt» - Summary
-------
Summary of Stack Gas Parameters and Test Results
Air Emissions Screening Test
Chemical Lime Company - Alabaster, Alabama
US EPA Test Method 26A - HCI
Kiln No. 1 Scrubber Stack
Page 1 of 2
Pnatte
r
Pbar
vm
A_1/2
Ap
cosfo) * Ap1/z
AH
Tm
Ts
V|c
C02
02
N2
cp
0
Dn
An
Vm(std)
Qm
PS
BWS
Bws(sat)
Vwstd
1-Bws
Md
M8
v,
Vsa
A
Qa
Qs
Qs
I
RUN NUMBER
RUN DATE
RUN TIME
MEASURED DATA
Stack Static Pressure, inches H2O
Meter Box Correction Factor
Barometric Pressure, inches Hg
Sample Volume, ft3
Average Square Root Ap, (in. H2O)1/2
In Flow Direction
In Axial Direction
Avg Meter Orifice Pressure, in. H2O
Average Meter Temperature, °F
Average Stack Temperature, °F
Condensate Collected, ml
Carbon Dioxide content, % by volume
Oxygen content, % by volume
Nitrogen content, % by volume
Pitot Tube Coefficient
Sample Run Duration, minutes
Nozzle Diameter, inches
CALCULATED DATA
Nozzle Area, ft2
Standard Meter Volume, ft3
Standard Meter Volume, m3
Average Sampling Rate, dscfm
Stack Pressure, inches Hg
Moisture, % by volume
Moisture (at saturation), % by volume
Standard Water Vapor Volume, ft3
Dry Mole Fraction
Molecular Weight (d.b.), Ib/lb-mole
Molecular Weight (w.b.), Ib/lb-mole
Stack Gas Velocity, ft/s
In Flow Direction
In Axial Direction
Stack Area, ft2
Stack Gas Volumetric flow, acfrn
Stack Gas Volumetric flow, dscfm
Stack Gas Volumetric flow, dscmm
Isokinetic Sampling Ratio, %
O-M26A-1
3/27/98
0909-1028
-0.46
1.000
29.50
41.934
0.7168
0.6208
1.56
76.4
137
NA
20.00
10.00
70.0
0.84
62.5
0.250
0.000341
40.839
1.156
0.653
29.47
NA
18.2
NA
0.818
31.60
29.13
42.9
37.2
18.35
40,913
29,165
826
104.5
O-M26A-2
3/27/98
1140-1255
-0.43
1.000
29.50
39.880
0.6911
0.5989
1.44
86.7
137
202.9
20.00
10.0
70.0
0.84
62.5
0.250
0.000341
38.098
1.079
0.610
29.47
20.0
18.4
9.551
0.816
31.60
29.09
41.4
35.9
18.35
39,509
28,053
794
101.4
O-M26A-3
3/27/98
1423-1538
-0.44
1.000
29.50
40.380
0.6914
0.6005
1.44
88.7
137
207.9
20.00
10.00
70.0
0.84
62.5
0.250
0.000341
38.431
1.088
0.615
29.47
20.3
18.4
9.786
0.816
31.60
29.09
41.4
36.0
18.35
39,616
28.136
797
102.2
Average
-0.44
1.000
29.50
40.731
0.6998
0.6067
1.48
83.9
137
205.4
20.0
10.0
70.0
0.84
63
0.250
0.000341
39.123
1.108
0.626
29.47
20.2
18.4
9.668
0.816
31.60
29.10
41.9
36.3
18.35
40,013
28,451
806
102.7
E:\iO12.002\Alabaste.r\Data\M26a-ouLxU - Sunrary
-------
Summary of Stack Gas Parameters and Test Results
Air Emissions Screening Test
Chemical Lime Company - Alabaster, Alabama
US EPA Test Method 26A - HCI
Kiln No. 1 Scrubber Stack
Page 2 of 2
FW,
Cppmvd
EHC.
Fw
Cppnwd
EC,
Fw,
Cppmvd
ENKM
Fw,
Cppmvd
EA,
Fw,
Cppmvd
EC.
Fw,
Cppmvd
EM,
Fw,
Cppmvd
EK
Fw,
Cppmvd
EN.
RUN NUMBER
RUN DATE
RUN TIME
EMISSIONS DATA
Chlorides as HCL
Target Catch, mg
Formula Weight, Ib/lb-mol
Concentration, ppm by volume
Emission Rate, Ib/hr
Chlorides as Cl
Target Catch, mg
Formula Weight, Ib/lb-mol
Concentration, ppm by volume
Emission Rate, Ib/hr
Ammonia as NH..
Target Catch, mg
Formula Weight, Ib/lb-mol
Concentration, ppm by volume
Emission Rate, Ib/hr
Aluminum, Al
Target Catch, ug
Formula Weight, Ib/lb-mol
Concentration, ppm by volume
Emission Rate, Ib/hr
Calcium. Ca
Target Catch, ug
Formula Weight, Ib/lb-mol
Concentration, ppm by volume
Emission Rate, Ib/hr
Magnesium. Mg
Target Catch, ug
Formula Weight, Ib/lb-mol
Concentration, ppm by volume
Emission Rate, Ib/hr
Potassium. K
Target Catch, ug
Formula Weight, Ib/lb-mol
Concentration, ppm by volume
Emission Rate, Ib/hr
Sodium. Na
Target Catch, ug
Formula Weight, Ib/lb-mol
Concentration, ppm by volume
Emission Rate, Ib/hr
O-M26A-1 O-M26A-2 O-M26A-3
3/27/98 3/27/98 3/27/98
0909-1028 1140-1255 1423-1538
1.70
36.47
0.968
0.160
1.65
35.45
0.968
0.156
0.25
18.04
0.288
0.0236
#N/A
26.98
#N/A
#N/A
#N/A
40.08
#N/A
#N/A
#N/A
24.31
#N/A
#N/A
#N/A
39.10
#N/A
#N/A
#N/A
22.99
#N/A
#N/A
2.18
36.47
1.33
0.212
2.12
35.45
1.33
0.206
0.35
18.04
0.433
0.0341
(27.0)
26.98
(0.0223)
(0.00263)
233.00
40.08
0.130
0.0227
45.80
24.31
0.0420
0.00446
78.9
39.10
0.0450
0.00768
119.0
22.99
0.115
0.0116
1.70
36.47
1.03
0.164
1.65
35.45
1.03
0.160
0.21
18.04
0.257
0.0203
#N/A
26.98
#N/A
#N/A
#N/A
40.08
#N/A
#N/A
#N/A
24.31
#N/A
#N/A
#N/A
39.10
#N/A
#N7A
#N/A
22.99
#N/A
#N/A
Average
1.86
36.47
1.11
0.179
1.81
35.45
1.11
0.174
0.27
18.04
0.326
0.0260
(27.0)
26.98
(0.0223)
(0.00263)
233.0
40.08
0.130
0.0227
45.8
24.31
0.0420
0.00446
78.9
39.10
0.0450
0.00768
119.0
22.99
0.115
0.0116
() - Not Detected
E:V012.0QZVAIataMta.rtDiMM26frouL>(i* - Sunmwy
-------
Example Calculations
Chemical Lime Company- Alabaster, Alabama
US EPA Method 23-PCDD/PCDF
(Using Data from Run M23-I-3)
Note: Discrepancies may exist between the computer generated reported results, which use
more significant figures, and the values manually calculated from the displayed values.
1. Volume of dry gas sampled corrected to standard conditions of 68 °F, 29.92 in. Hg, ft3.
m(8td)
bar
AH
13.6
460 + t.
m(,td)
= (17.64)(91.987)(1.021)
29.5 +
0.935
13.6
( 460 + 101.77 J
V , = 87.202 dscf
m(std)
2. Volume of dry gas sampled corrected to standard conditions of 68 °F, 29.92 in. Hg, m3
' = Vmstd(0.028317)
m(std)
= (87.202)(0.028317)
> = 2'469 dscm
3. Volume of water vapor at standard conditions, ft3.
yw(,td) = 0.04707VU
Vw(,td) = (0-04707) (320.5)
Vw(std) = 15-086 scf
-------
4. Moisture content in stack gas.
V
B = v«(std)
™ (V + V \
lvm(std) vw(std)J
B = 15.086
87.202 + 15.086
_ = 0.1475
5. Dry molecular weight of stack gas, Ib/lb-mol.
Md = 0.44 (%CO2) + 0.32 (%O2) + 0.28(%N2+%CO)
Md = 0.44(20.0) + 0.32(10.0) + 0.28(70 + 0)
Md = 31.60 Ib/lbmol
6. Molecular weight of stack gas, Ib/lb-mol.
H = Md(l -BJ + 18(BWS)
Ms = 31.60(1-0.1475) + 18(0.1475)
M. = 31.60(0.8525) + 18(0.1475)
Ms = 26.939 + 2.664
Ms = 29.59 Ib/lbmol
-------
7. Absolute stack gas pressure, in. Hg.
p = p
rs rbar
. 29.5
* static
13.6
13.6
Ps = 29.16 inches Hg
8. Stack velocity at stack conditions, rps.
v = 85.49 C
avg
ts + 460
M. P.
s s
v, = (85.49)(0.84)(0.6865)
(775+460)
(29.59) (29.16)
vs = 58.98 rps
9. Isokinetic Variation.
W (' -
(87.202) (775+460) (17.32)
(58.98) (0.250)2 (180) (29.16) (1-0.1475)
= 113.1
-------
10. Stack gas volumetric flow rate at stack conditions, acfrn.
Qs = (60) (A) (vs)
Qs = (60) (25.00) (58.98)
Qs = 88,472 acfm
11. Dry stack gas volumetric flow rate at standard conditions, dscfin.
= 17-64 Qs £ (1 -Bws)
n = (17.64) (88,472) ——(1-0.1475)
^s(std) v j \ ' 775 + 460
Qs(std) = 31'410 dscfm
12. Dry stack gas volumetric flow rate at standard conditions, dscmm.
(0.028317)
QS(std)m'/,nin = 889 dscmm
-------
13. Pollutant (2378 TCDD) concentration, ng/dscm.
ng/dscm = -—-
m(std)m
.. < 0.003
ng/dscm =
& 2.469
ng/dscm = < 0.00121 ng/dscm
14. Pollutant (2378 TCDD) concentration, ng/dscm adjusted to 7 percent oxygen.
ng/dscm@7%O, = (ng/dscm)
& ^ 2 (20.9 - %02)
ng/dscm@7%O, = (< 0.00121) —
& ° 2 V (20.9 - 10.0)
ng/dscm@7%O2 = < 0.00155 ng/dscm@7%O2
15. Pollutant (2378 TCDD) emission rate, ug/hr.
= (60) (ng) (Qs(std))
do3) (vm(std))
_ (60) (< 0.003) (31,410)
(103) (87.202)
Atg/hr = < 0.0648 //g/hr
-------
APPENDIX D
CALIBRATION DATA
-------
PACIFIC ENVIRONMENTAL SERVICES.INC.
4700 Duke Drive,
Suite 150
Mason, Ohio
Phone: (513) 398-2556
Fax: (513)3983342
www.pes.com
TEMPERATURE SENSOR CALIBRATION DATA
FOR STACK THERMOCOUPLES
THERMOCOUPLE NUMBER:
T7D
DATE:
12/22/97
BAROMETRIC PRES.(ln.Hg):
AMBIENT TEMP. °F:
29.52
74
REFERENCE:
Mercury-in-glass:
Other:
"CALIBRATOR:
ASTM-3F
G. Gay
Reference
point
number
1
2
3
4
Source3
(Specify)
Ambient Air
Cold Bath
Hot Bath
Hot Oil
Reference
Thermometer
Temperature,°F
73
35
205
352
Thermocouple
Potentiometer
Temperature,°F
75
38
206
355
Temperature
Difference,13
%
0.38
0.61
0.15
0.37
aType of calibration used.
b(ref. temp.°F+460Wtest thermometer temp.°F+460) X100
ref temp,°F+460
100<1.5%
Comments:
STACK THERMOCOUPLE CALIBRATION FORM
1998 Yearly Calibration
-------
PACIFIC ENVIRONMENTAL SERVICES.INC.
4700 Duke Drive,
Suite 150
Mason, Ohio
Phone: (513) 398-2556
Fax: (513) 3983342
www.pes.com
TEMPERATURE SENSOR CAUBRATION DATA
FOR STACK THERMOCOUPLES
THERMOCOUPLE NUMBER:
7D
DATE:
12/23/97
BAROMETRIC PRES.(ln.Hg):
AMBIENT TEMP. °F:
29.52
74
REFERENCE:
Mercury-in-glass:
Other:
"CALIBRATOR:
ASTM-3F
G. Gay
Reference
point
number
1
2
3
4
Source8
(Specify)
Ambient Air
Cold Bath
Hot Bath
Hot Oil
Reference
Thermometer
Temperature,°F
74
40
206
340
Thermocouple
Potentiometer
Temperature,°F
74
41
205
341
Temperature
Difference,"
%
0.00
0.20
0.15
0.13
"Type of calibration used.
"fref. temp.°F+460Wtest thermometer temp.°F+460^ X100
reftemp,°F+460
100<1.5%
Comments:
STACK THERMOCOUPLE CALIBRATION FORM 1998 Yearly Calibration
-------
TEMPERATURE SENSOR CALIBRATION FORM
Temperature Sensor No.
Ambient Temp. °F
,
Sensor Type K ~
Length
Barometric Pressure, "Hg
«/
Reference Temp. Sensor:
Date
^'\%'C|V
/,
•'
Ref.
Point
No.
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
Temp.
Source
£1
•S/W?-
M A.
%i'
Temp. °F
Ref.
Sensor
ys
7-f
2,0-6
Test
Sensor
33
•7i"
2.0*
Temp.
Diff. %
o
. IB7
o
Within
Limits
Y/N
Y
Y
Y
Calibrated
By
f\W^>
m^
Xu\
% Temp Diff
p'
(Ref ' Teiap + 40) " ( TeSt
460)
,
(JJef . Terap. + 460)
100 S 1.5 %
-------
TEMPERATURE SENSOR CALIBRATION FORM
Temperature Sensor No. PGM -\ P Sensor Type <-TC Length _J
Ambient Temp. °F 14 Barometric Pressure, "Hg
Reference Temp. Sensor:
Date
^-)&-*ijr
u
cf
Ref.
Point
No.
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
Temp.
Source
\C<£.
&*£'
wlo*
Temp. °F
Ref.
Sensor
33
7^-
Zo*
Test
Sensor
S^
7t
•Z-l O
Temp.
Diff. %
.4-a*.
0
• til
Within
Limits
Y/N
N
V
V(
Calibrated
By
X^
iv^"B
>i^
% Temp. Diff = (J?ef •
460) " < rest
(flef . Temp. + 460)
46°)
x 100 s 1 5
D
-------
c
TEMPERATURE SENSOR CALIBRATION FORM
DC-M-Oof
Temperature Sensor No.
Ambient Temp. °F 7
Sensor Tvne
Reference Temp. Sensor:
Length I
Barometric Pressure, "Kg
Date
VZo-iY
'1
if
Ref.
Point
No.
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
Temp.
Source
{C<£
{•KO
^-
$u&
% Temp Diff =
Temp + 460) - ( Test Temp. + 460) -nn . ,. .
(Ref ^ reng?> ^ 46Q) x 100 s 1.5 %
-------
TEMPERATURE SENSOR CALIBRATION FORM
Temperature Sensor No. h\vb-
Ambient Temp. °F -7 £
Sensor Type
Length g
Reference Temp. Sensor:
Barometric Pressure, "Hg
Date
&-ZD.W
"
n
Ref.
Point
No.
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
Temp.
Source
»c«£.
*£*_'
VU^
,
Temp. °F
Ref.
Sensor
*S
1C,
z^c.
Test
Sensor
34-
7^
^>5-
^
Temp.
Diff. %
o
Within
Limits
Y/N
Calibrated
By
% Temp Diff
•s ^ciii^. i/xj-J.
40) " ( TeSt
460>
(Ref. Temp. +
100 5 1.5 %
-------
T7D
PACIFIC ENVIRONMENTAL SERVICES, INC.
4700 Duke Drive,
Suite 150
Mason, Ohio 45040
Phone:(513)398-2556
Fax (513) 398-3342
www.pes.com
Pilot Tube Number: T7D Date:
Effective Length: 84" Calibrated By:
Pilot Tube Openings Damaged? YES | NO ]
Pitol Tube Assembly Level? | YES | NO
a , = 0 °« 10°) a 2 =
P, = 1 °(<5°) p. =
Y= 0 9= 1 A =
z = A sin Y = 0 cm (in.) 0.32 cm ( < 1/8 in.)
w = A sin 6 = 0.017 cm (in.) 0.08 cm ( < 1/32 in.)
PA = 0.487 cm (in.)
12/22/97
S. Simon
1 °(< 10°)
3 °(<5°)
0.973
PB =
0.486
cm (in.)
rV
0.375
cm (in.)
......;,^S«.Mii*S:
(c)
(a)
ThB types or fsos-opsnlngmlsallonment shown above wil not affect thebaselne value of Cp(s) so
long as °S«nd °SI» less than or equal to 1O*, O, and Oz t» less than or equal to 5°, z Is lass than or
equal to O.32 cm (1/8 In.), and w is less than or equal to O.OB am(1/32 in.) (reference-! 1.O In
Pitot Tube Calibration Form
1998 Yearly Calibration
-------
7D
PACIFIC ENVIRONMENTAL SERVICES, INC.
4700 Duke Drive,
Suite 150
Mason, Ohio 45040
Phone: (513) 398-2556
Fax (513) 398-3342
www.pes.com
Pilot Tube Number:
Effective Length:
7D
84.5"
Date: 12/23/97
Calibrated By:
YES
Pilot Tube Openings Damaged?
Pilot Tube Assembly Level? I YES |
a , . 3 °« 10°)
Pi -
Y=
NO
1
1
(«5°)
e
(32 =
z = A sin Y -
w = A sin 6 =
0.016
cm (in.) 0.32 cm ( < 1/8 in.)
cm (in.) 0.08 cm ( < 1/32 in.)
0.466 cm (in.)
S. Simon
0.931
'(< 10°)
Tha typ«aorfaca-opanlngma>a1lgrm*r* shown abov* wllnct affect tha baaaln* vmkimot Cp(s) mo
tore mm «,«nd«SI» !••• than or «qMBl to 1OVQ, »nd a, !•!••• than cr*qu>lto ST. z to IBM than or
•qua! to Q32 cm (1/8 In.), and w to la aa than or equal toO.OB em(1/32 In.) (rafaranoal 1.O h
Pitot Tube Calibration Form
1998 Yearly Calibration
-------
•aro~tr»c Pr-aura 29.73
REFERENCE HETER CALIBRATION
ENGLISH REFERENCE NETER UNITS
oS.*"™ *
)a» Prasaura
. (in. H20)
6.00 -6.60
24.00 -6.60
8.00 -6.60
10.00
35.00
16.50
12.50
14.00
58.50
16.50
42.00
66.50
15.30
13.50
35.00
411.42* 421.233
iS SS
-4.00 464.1*7
•2.80 479.992 489.698
•2.80 489.698 500.594
-2.80 500.594 546.063
-1.60 574.496 583.672
-1.60 590.619 614.123
-1.60 614.123 651.520
•1.30 651.520 657.572
•1.30 657.572 663.065
•1.30 663.065 677.274
9.809
gg?
479.992 15.845 rrl l .' lJS
9.706
10.896
4S.469
9.176
23.504
37.397
6.052
5.493
14.209
a
Signature
78.0
78.0
78.0
79.0
80.0
80.0
81.0
82.0
32.0
78.0 601.625 611.270
78.0 611.270 622.061
79.0 622.061 667.125
79.0 695.390 704.530
80.0 711.429 734.785
81.0 734.785 771.901
82.0 771.901 777.994
82.0 777.994 783.400
32.0 783.400 797.515
ss
^'SS 2*2 I'011 °*000 i"a»
9.808 77.0 1.015 0 004 1 197
Max Yds - Nfn Yds -0.007489914 Must bt no grtatar than 0.030
Avaragt Yds -1.011058546 Must ba batilaan fl.9Sto lios
«'»S S'2 I'£5 °*009 °-926
15*660 770 0*999 I0'003 0'924
Max Yds - Nfn Y* -0.014197179 Must ba'no graatar°than 0.030
Avaraga Yda -1.004786738 Must ba batwaan 0.95 to 1*05
9.645 77.0 1.003 Q 002 0 754
10.791 77.0 0.999 .fl'ool Q 7W
«ntL rr n . Ill u.uu* v.133
.06* 77.0 1.001 0.000- 0 7S2
Max Tds • Mfn Yds - 0.00338145 Must ba no graatar than 0.030
Avarag. Yds -1.000808891 Must ba batStan 0^95 M t.05
.Mi? 2-2 '-M* 0.000 0.541
(7.0 1.003 0.000 O.S43
77.0 1.003 0.000 0 545
Yd* 4.000835063 Must ba noTaatar than 0 030
Yds -1.003302203 Must ba batMaan 0.95 to ll»
Si/lA y%* n -I*AM« J«m I 0*396
.•*uo fo.u J.994 *d 01 ft ft ton
14.115 78.0 1.003 -flloo! 0393
Max
r u . a ,,
-------
REFERENCE METER CALIBRATION
ENGLISH REFERENCE METER UNITB
Barometric Pressure 29.82
Meter Yw 1.00000
K ( deg R/Inches Kg) 17.64
DGM Serial i
Bate
6841495
10/5/97
FUenaMt
Revised:
FiVDATAFILE\CALIBRAT\CAL NENU.DSKNDGM REF.
06/08/95
TIM
(•In)
20.50
5.00
13.00
8.50
27.50
26.50
14.00
15.50
12.50
23.50
17.50
15.00
32.00
35.CO
15.00
Dry Gas Meter (DGM)
Pressure Meter Readings VoluM
(In. H20) Initial Final
•8.000 742.719 766.193
•8.000 768.193 774.402
-8.000 774.402 790.575
Tetperature
Initial Final
(cubic feet) (deg F) (deg F)
25.474 78.0 79.0
6.209 79.0 79.0
16.173 79.0 79.0 703.325
Vet Test Meter (UTM)
Meter Readings Voluw
Initial Final (cubic feet)
671.890
697.180
697.180
703.325
719.309
25.290
6.145
15.984
Max Yds
DON
Teap Coefficient
(deg F) Yds
77.0 1.016
77.0 1.013
77.0 1.012
Coefficient
Variation
Yds-(Avg.Yds)
0.002
0.000
•0.002
Flow
Rate
(CFN)
1.208
1.204
1.204
NIn Yds •0.003626886 Must be no greater than 0.030
-5.400 790.575 798.821 8.246 79.0
-5.400 798.821 825.423 26.602 79.0
-3.400 825.423 850.983 25.560 80.0
-3.800 850.983 861.899 10.916 81.0
-3.800 861.899 873.960 12.061 81.0
-3.800 .953.219 962.970 9.751 86.0
-2.400 962.970 976.611 13.641 86.0
-2.400 976.611 986.740 10.129 87.0
-2.400 986.740 995.413 8.673 87.0
•1.600 995.413 1008.596 13.183 88.0
•1.600 1008.596 1022.986 14.390 89.0
•1.600 1022.986 1029.158 6.172 89.0
79.0 719.309 727.485
80.0 727.485 753.809
81.0 753.809 779.025
81.0 779.025 789.820
82.0 789.820 801.740
86.0 879.651 889.205
87.0 889.205 902.599
87.0 902.599 912.545
88.0 912.545 921.069
89.0 921.069 934.025
89.0 934.025 948.175
90.0 948.175 954.255
Average Yda •1.013636253 Must be between 0.95 to 1.05
8.176 77.0 1.009 0.001 0.942
26.324 77.0 1.008 0.000 0.938
25.216 77.0 1.006 -0.001 0.932
Max Yds - NIn Yds •0.002262496 Must be no greater than 0.030
Average Yds •1.007525980 Must be between 0.95 to 1.05
10.795 77.0 1.006 0.001 0.755
11.920 77.0 1.006 0.001 0.753
9.554 78.0 1.004 -0.001 0.747
Max Yds • NIn Yds -0.002245979 Must be no greater then 0.030
Average Vda •1.005164785 Must be between 0.95 to 1.05
13.394 78.0 1.003 . -0.001 0.557
9.946 78.0 1.004 0.000 0.556
8.524 78.0 1.006 0.002 0.556
Max Yds - NIn Yds -0.002785363 Must be m greater than 0.030
Average Yds -1.004591811 Must be between 0.95 to 1.05
12.956 78.0 1.006 -0.002 0.396
14.150 78.0 1.007 0.000 0.395
6.080 78.0 1.010 0.002 0.396
Max Yds - NIn Yds -0.004205886 Must be no greater than 0.030
Average Yds •1.007822494 Must be between 0.95 to 1.05
Overall Average Yds •1.007748265
*rtlfy that the above Dry Gas Meter was calibrated In accordance with E.P.A. Method 5 . paragraph 7.1 sCFR 40 Part 60,
ng the Precision Wet Test Meter f 11AE6, which In turn was calibrated using the Anerlcan Bell Prover f 3785.
tlflcate f F107, whJcK la traceable to the National Bureau of Standards (N.I.S.T.).
Signature
Date
-------
PACIFIC ENVIRONMENTAL SERVICES, INC.
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Posttest Dry Gas Meter Calibration Form (English Units)
Pretest Calibration Factor
System Vacuum Setting, (in Hg)
Reference Meter Correction Factor
Date: 5/2/98 PD*. in Hg
1.000
12
1.0077
29.94 Calibrator
D. Holzschuh
Meter Box No.
MB-15
AH = 1.41
Trial
1
2
3
Duration
(min)
8
8
11
Dry Gas Meter
Initial
(ft3)
776.09
781.709
787.439
Final
(ft3)
781.709
787.439
795.344
Net
(ft3)
5.619
5.730
7.905
Initial, Inlet
CF)
71
73
73
Final, Inle
(°F)
73
73
73
Avg. Inlet
CF)
72
73
73
Initial, Outlet
CF)
69
70
71
Final, Outlet
CF)
70
71
71
Avg. Outlet
CF)
69.5
70.5
71
Trial
1
2
3
Reference Meter
Gas Volume
Initial
(ft3)
343.209
348.9
354.597
Final
(ft3)
348.9
354.597
362.414
Net
(ft3)
5.691
5.697
7.817
Meter Temperature
Initial
CF)
72
72
72
Final
CF)
72
72
72
Avg.
CF)
72
72
72
Meter Box
Correction
Factor
Y
1.015
0.998
0.993
Reference
Orifice Press
AH0
(in. H20)
1.56
1.56
1.56
15J0137.XIS
PostTest50298
6/10798
-------
2 Of 2
7 PACIFIC ENVIRONMENTAL SERVICES. INC.
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919)941-0333 FAX: (919) 941-0234
AH- 2.0
Trial
1
2
3
Trial
Duration
(min)
9
7
7
Dry Gas Meter RMB-15
Gas Volume
Initial
(ft3)
13.863
20.884
26.372
Final
(ft3)
20.884
26.372
31.871
Net
(ft3)
7.021
5.488
5.499
Meter Temperatures
Initial, Inlet
cn
87
90
90
Final. Inlet
91
92
93
Avg. Inlet
89
91
91.5
Initial, Outlet
83
84
84
inal, Outie
CF)
83
84
84
Avg. Outlet
CF)
83
84
84
Trial
1
2
3
Reference Meter
Gas Volume
Initial
(ft3)
97.749
104.591
109.929
Final
(ft8)
104.591
109.929
115.281
Net
(ft3)
6.842
5.338
5.352
Meter Temperature
Initial
CF)
73
73
73
Final
CF)
73
73
74
Avg.
CF)
73
73
73.5
Meter Box
Correction
Factor
T
1.001
1.002
1.002
Reference
Orifice Press
AH0
(in. H20)
1.90
1.89
1.88
AH = 4.0
Trial
1
2
Trial
Duration
(min)
6.5
15.5
Dry Gas Meter RMB-15
Gas Volume
Initial
(ft3)
32.371
39.484
Final
(ft3)
39.484
56.484
Net
(ft3)
7.113
17.000
Meter Temperatures
Initial, Inlet
CF)
92
93
Final, Inlet
CF)
94
97
Avg. Inlet
CF)
93
95
Initial, Outlet
CF)
85
87
inal, Outie
CF)
85
87
Avg. Outlet
CF)
85
87
Trial
1
2
Reference Meter
Gas Volume
Initial
(ft3)
15.775
22.732
Final
(ft3)
22.732
39.287
Net
(ft3)
6.957
16.555
Meter Temperature
Initial
CF)
73
73
Final
CF)
74
73
Avg.
CF)
73.5
73
Meter Box
Correction
Factor
y
1.004
1.005
Reference
Orifice Press
AH0
(in. H2O)
1.92
1.92
Calibration Results
AFT
AHO
0.50
0.75
1.0
2.0
4.0
0.999
0.996
1.000
1.002
1.004
1.86
1.90
1.92
1.89
1.92
Dry Gas Meter RMB-15 on 10/13/97
Meter Box Calibration Factor
Meter Box Reference Orifice Pressure
• Two Trial Average
1.000
1.90
15 10137.xls
Printed: 6/10/98
-------
1of2
PACIHC ENVIRONMENTAL SERVICES, INC.
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919)941-0333 FAX: (919) 941-0234
Date:
10/13/97
29.86
Calibrator MMD
Meter Box No.: RMB-15
Reference Meter Correction Factor. 1.0077 (10/5/97)
AH- 0.5
Trial
1
2
3
Trial
.Duration
(min)
15
13
12
Dry Gas Meter RMB-15
Gas Volume
Initial
(fl3)
48.833
54.722
59.821
Final
(fl3)
54.722
59.821
64.544
Net
(^
5.889
5.099
4.723
Meter Temperatures
Initial, Inlet
CF)
73
78
80
Final, Inlet
CF)
77
80
83
Avg. Inlet
en
75
79
61.5
Initial, Outlet
72
74
76
inal. Outta
en
75
75
77
Avg. Outlet
en
73.5
74.5
76.5
Trial
1
2
3
Reference Meter
Gas Volume
Initial
(ft3)
34.044
39.829
44.843
Final
(ft3)
39.829
44.843
49.463
Net
(ft3)
5.785
5.014
4.620
Meter Temperature
initial
CF)
70
71
71
Final
CF)
70
70
71
Avg.
CF)
70
70.5
71
Meter Box
Correction
Factor
T
0.997
1.001
0.999
Reference
Orifice Press
AHo
(in-HjO)
1.86
1.86
1.86
AH = 0.75
Trial
1
2
3
Trial
Duration
(min)
8
21
13
Dry Gas Meter RMB-15
Gas Volume
Initial
^
69.524
73.327
83.322
Final
(ft3)
73.327
83.322
89.571
Net
(ft3)
3.803
9.995
6.249
Meter Temperatures
Initial, Inlet
CF)
74
77
78
Final, Inlet
74
83
82
Avg. Inlet
CF)
74
80
80
Initial. Outlet
77
76
78
inal, Outle
CF)
75
77
74
Avg. Outlet
CF)
76
76.5
76
Trial
1
2
3
Reference Meter
Gas Volume
Initial
(ft3)
54.365
58.108
67.912
Final
(ft3)
58.108
67.912
74.036
Net
(ft3)
3.743
9.804
6.124
Meter Temperature
Initial
CF)
72
72
73
Final
CF)
72
73
73
Avg.
CF)
72
72.5
73
Meter Box
Correction
Factor
T
0.996
0.997
0.995
Reference
Orifice Press
AH0
(in. H20)
1.91
1.91
1.88
AH = 1.0
Trial
1
2
3
Trial
Duration
(min)
19
8
16
Dry Gas Meter RMB-15
Gas Volume
Initial
(ft3)
89.777
100.214
104.614
Final
(ft3)
100.214
104.614
113.404
Net
(ft3)
10.437
4.400
8.790
Meter Temperatures
Initial, Inlet
CF)
62
85
85
Final, Inlet
CF)
86
87
88
Avg. Inlet
CF)
84
86
86.5
Initial, Outlet
CF)
79
81
82
inal, Outle
CF)
80
81
83
Avg. Outlet
CF)
79.5
81
82.5
Trial
1
2
3
Reference Meter
Gas Volume
Initial
(ft3)
74.254
84.440
88.743
Final
(ft3)
84.44
88.743
97.302
Net
(ft3)
10.186
4.303
8.559
Meter Temperature
Initial
CF)
73
73
73
Final
CF)
73
73
73
Avg.
CF)
73
73
73
Meter Box
Correction
Factor
T
0.997
1.002
1.000
Reference
Orifice Press
AH0
(IruHjO)
1.92
1.91
1.92
15 10137 jcls
Printed: 6/10/98
-------
PACIFIC ENVIRONMENTAL SERVICES, INC.
Centra! Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Posttest Dry Gas Meter Calibration Form (English Units)
Pretest Calibration Factor
System Vacuum Setting, (in Hg)
Reference Meter Correction Factor
Date: 5/2/98 P^, in Hg
1.021
16
1.0077
29.94 Calibrator
D. Holzschuh
Meter Box No.
MB-10
AH= 1.41
Trial
1
2
3
Duration
(min)
15
8
8
Dry Gas Meter
Initial
(ft3)
902.1
912.624
917.493
Final
(ft3)
912.624
917.993
923.154
Net
(ft3)
10.524
5.369
5.661
Initial, Inlet
(°F)
75
76
76
Final, Inle
(°F)
76
76
76
Avg. Inlet
(°F)
75.5
76
76
Initial, Outlet
(8F)
74
74
74
Final, Outlet
CF)
74
74
74
Avg. Outlet
(°F)
74
74
74
Trial
1
2
3
Reference Meter
Gas Volume
Initial
(ft3)
320.645
331.244
336.545
Final
(ft3)
331.244
336.545
341.865
Net
(ft3)
10.601
5.301
5.32
Meter Temperature
Initial
(°F)
75
72
73
Final
(°F)
75
73
73
Avg.
(°F)
75
72.5
73
Meter Box
Correction
Factor
T
1.011
0.996
0.947
Reference
Orifice Press
AH0
(in. H20)
1.59
1.79
1.78
10_09017.xls
PostTest050298
6/10/98
-------
2 of 2
7 PACIFIC ENVIRONIIEKTAL SERVICES. INC.
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park. North Carolina 27709-2077
(919)941-0333 FAX: (919) 941-0234
AH - 2.0
Trial
1
2
3
Trial
Duration
(min)
10
10
10
Dry Gas Meter MB-10
Gas Volume
Initial
(ft3)
55.668
63.519
71.182
Final
(ft3)
63.519
71.182
78.845
Net
(ft3)
7.651
7.663
7.663
Meter Temperatures
Initial. Inlet
CF)
84
86
86
Final. Inlet
CF)
86
86
87
Avg. Inlet
CF)
85
86
86.5
Initial, Outlet
CF)
81
81
81
inal, Outte
CF)
81
81
81
Avg. Outlet
CF)
81
81
81
Trial
1
2
3
Reference Meter
Gas Volume
Initial
(ft3)
662.729
670.472
678.244
Final
(ft3)
670.472
678.244
686.010
Net
(ft3)
7.743
7.772
7.766
Meter Temperature
Initial
CF)
78
78
78
Final
CF)
78
78
78
Avg.
CF)
78
78
78
Meter Box
Correction
Factor
Y
1.021
1.025
1.024
Reference
Orifice Press
AH,
(In-HjO)
1.87
1.86
1.86
AH = 4.0
Trial
1
2
3
Trial
Duration
(min)
8
8
8
Dry Gas Meter MB-10
Gas Volume
Initial
(ft3)
79.058
86.620
94.185
Final
(ft3)
86.620
94.185
101.754
Net
(ft3)
7.562
7.565
7.569
Meter Temperatures
Initial, Inlet
CF)
85
87
89
Final. Inlet
CF)
88 •
89
89
Avg. Inlet
CF)
86.5
88
89
Initial, Outlet
CF)
81
82
82
inal.Outte
CF)
82
82
82
Avg. Outlet
CF)
81.5
82
82
Trial
1
2
3
Reference Meter
Gas Volume
Initial
(ft3)
686.208
693.895
701.558
Final
(ft3)
693.895
701.558
709.244
Net
(ft3)
7.687
7.663
7.686
Meter Temperature
Initial
CF)
78
78
78
Final
CF)
78
78
78
Avg.
CF)
78
78
78
Meter Box
Correction
Factor
y
1.023
1.021
1.025
Reference
Orifice Press
AH0
(in. H20)
2.44
2.45
2.43
Calibration Results
AH
0.50
0.75
1.0
2.0
4.0
T | AH«
1.020 1.73
1.020 1.79
1.020 1.78
1.023 1.86
1.023 2.44
Dry Gas Meter MB-10 on 09/01/97
Meter Box Calibration Factor
Meter Box Reference Orifice Pressure
1.021
1.92
10 09017jcls
Printed: 6/10/98
-------
1of2
PACIFIC ENVIRONMENTAL SERVICES. iNC.
Central Pa* West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Date:
9/1/97
30.16
Calibrator Tom McDonald
Meter Box No.: MB-10
Reference Meter Correction Factor. 1.0049 (8/28/96)
AH - 0.5
Trial
1
2
3
Trial
Duration
(min)
19
19
19
Dry Gas Meter MB-10
Gas Volume
Initial
(ft3)
994.409
1001.982
1009.513
Final
1001.982
1009.513
1017.050
Net
<«*)
7.573
7.531
7.537
Meter Temperatures
Initial, Inlet
74
77
80
Final, Inlet
78
80
81
Avg. Inlet
CF)
76
78.5
80.5
Initial, Outlet
73
75
77
inal.Outte
CF)
75
77
78
Avg. Outlet
en
74
76
77.5
Trial
1
2
3
Reference Meter
Gas Volume
Initial
(ft3)
600.523
608.185
615.801
Final
(ft3)
608.185
615.801
623.430
Net
(ft3)
7.662
7.616
7.629
Meter Temperature
Initial
CF)
72
74
76
Rnal
CF)
74
76
77
Avg.
CF)
73
75
76.5
Meter Box
Correction
Factor
Y
1.019
1.019
1.021
Reference
Orifice Press
AH0
(In-HzO)
1.71
1.74
1.74
AH = 0.75
Trial
1
2
3
Trial
Duration
(min)
15
15
15
Dry Gas Meter MB-10
Gas Volume
Initial
(ft3)
17.220
24.350
31.563
Final
^
24.350
31.563
38.780
Net
(ft3)
7.130
7.213
7.217
Meter Temperatures
Initial, Inlet
CF)
80
82
82
Final, Inlet
CF)
82
83
83
Avg. Inlet
CF)
81
82.5
82.5
Initial, Outlet
CF)
78
79
79
inal, Outte
CF)
79
79
81
Avg. Outlet
CF)
78.5
79
80
Trial
1
2
3
Reference Meter
Gas Volume
Initial
(ft3)
623.622
630.833
638.141
Final
(ft3)
630.833
638.141
645.425
Net
(ft3)
7.211
7.308
7.284
Meter Temperature
Initial
CF)
77
78
78
Final
CF)
77
78
78.5
Avg.
CF)
77
78
78.25
Meter Box
Correction
Factor
Y
1.020
1.021
1.018
Reference
Orifice Press
AH0
(in. H20)
1.82
1.77
1.79
AH= 1.0
Trial
1
2
3
Trial
Duration
(min)
10
10
10
Dry Gas Meter MB-10
Gas Volume
Initial
(«*)
38.946
44.490
50.050
Final
(ft3)
44.490
50.050
55.585
Net
^
5.544
5.560
5.535
Meter Temperatures
Initial, Inlet
CF)
81
83
84
Final, Inlet
CF)
83
84
84
•Avg. Inlet
CF)
82
83.5
84
Initial, Outlet
CF)
80
80
80
inal, Outle
CF)
80
80
80
Avg. Outlet
CF)
80
80
80
Trial
1
2
3
Reference Meter
Gas Volume
Initial
(ft3)
645.614
651.220
656.829
Final
(ft3)
651.22
656.829
662.435
Net
(ft3)
5.606
5.609
5.606
Meter Temperature
Initial
CF)
78
78
78
Final
CF)
78
78
78
Avg.
CF)
78
78
78
Meter Box
Correction
Factor
Y
1.019
1.018
1.023
Reference
Orifice Press
AH0
(in. H20)
1.79
1.78
1.78
10 09017.xls
Printed: 6/10/98
-------
APPENDIX E
TEST PARTICIPANTS
-------
-------
PROJECT PARTICIPANTS
Name
Affiliation
Responsibility
Michael L. Toney
Franklin Meadows
Frank J. Phoenix
Troy Abemathy
Paul Siegel
Gary Gay
Mike Maret
Cybelle Brockman
Eric Dithrich1
Terry Thomasson1
USEPA, Emission Measurement Center
Pacific Environmental Services, Inc.
Pacific Environmental Services, Inc.
Pacific Environmental Services, Inc.
Pacific Environmental Services, Inc.
Pacific Environmental Services, Inc.
Pacific Environmental Services, Inc.
Research Triangle Institute
APCC
APCC
Work Assignment Manager
Project Manager
Task Manager
Site Leader/Console Operator
Site Leader/Console Operator
Sampling Technician
Sampling Technician/Sample Recovery
Process Data Recorder
CEM Team Leader
CEM Sampling Technician
1 Subcontractor to Pacific Environmental Services, Inc.
-------
APPENDIX F
PROCESS DATA
Process data was collected by RTI personnel
under a separate work assignment.
-------
APPENDIX G
TEST METHODS
-------
Appendix G.I
EPA Method 1
-------
-------
EMISSION MEASUREMENT TECHNICAL INFORMATION CENTER
NSPS TEST METHOD
Method 1 - Sample and Velocity Traverses for Stationary Sources
1. PRINCIPLE AND APPLICABILITY
1.1 Principle. To aid in the representative measurement of
pollutant emissions and/or total volumetric flow rate from a
stationary source, a measurement site where the effluent stream is
flowing in a known direction is selected, and the cross-section of
the stack is divided into a number of equal areas. A traverse
point is then located within each of these equal areas.
1.2 Applicability. This method is applicable to flowing gas
streams in ducts, stacks, and flues. The method cannot be used
when: (1) flow is cyclonic or swirling (see Section 2.4), (2) a
stack is smaller than about 0.30 meter (12 in.) in diameter, or
0.071 m2 (113 in.2) in cross-sectional area, or (3) the measurement
site is less than two stack or duct diameters downstream or less
than a half diameter upstream from a flow disturbance.
The requirements of this method must be considered before
construction of a new facility from which emissions will be
measured; failure to do so may require subsequent alterations to
the stack or deviation from the standard procedure. Cases
involving variants are subject to approval by the Administrator,
U.S. Environmental Protection Agency.
2. PROCEDURE
2.1 Selection of Measurement Site. Sampling or velocity
measurement is performed at a site located at least eight stack or
duct diameters downstream and two -diameters upstream from any flow
disturbance such as a bend, expansion, or contraction in the stack,
or from a visible flame. If necessary, an alternative location may
be selected, at a position at least two stack or duct diameters
Prepared by Emission Measurement Branch EMTIC TM-001
Technical Support Division, OAQPS, EPA
-------
EMISSION MEASUREMENT TECHNICAL INFORMATION CENTER
NSPS TEST METHOD
downstream and a half diameter upstream from any flow disturbance.
For a rectangular cross section, an equivalent diameter (De) shall
be calculated from the following equation, to determine the
upstream and downstream distances:
2LW
e (L + W)
Eq. 1-1
Where
L = Length and W = width.
An alternative procedure is available for determining the
acceptability of a measurement location not meeting the criteria
above. This procedure,
determination of gas flow angles at the sampling points and
comparing the results with acceptability criteria, is described in
Section 2.5.
2.2 Determining the Number of Traverse Points.
2.2.1 Particulate Traverses. When the eight- and two-diameter
criterion can be met, the minimum number of traverse points shall
be: (1) twelve, for circular or rectangular stacks with diameters
(or equivalent diameters) greater than 0.61 meter (24 in.); (2)
eight, for circular stacks with diameters between 0.30 and 0.61
meter (12 and 24 in.); and (3) nine, for rectangular stacks with
equivalent diameters between 0.30 and 0.61 meter (12 and 24 in.) .
When the eight- and two-diameter criterion cannot be met, the
minimum number of traverse points is determined from Figure 1-1.
Before referring to the figure, however, determine the distances
from the chosen measurement site to the nearest upstream and
downstream disturbances, and divide each distance by the stack
Prepared by Emission Measurement Branch EMTIC TM-001
Technical Support Division, OAQPS, EPA
-------
EMTIC TM-001 EMTIC NSPS TEST METHOD Page 3
diameter or equivalent diameter, to determine the distance in terms
of the number of duct diameters. Then, determine from Figure 1-1
the minimum number of traverse points that corresponds: (1) to the
number of duct diameters upstream; and (2) to the number of
diameters downstream. Select the higher of the two minimum numbers
of traverse points, or a greater value, so that for circular stacks
the number is a multiple of 4, and for rectangular stacks, the
number is one of those shown in Table 1-1.
2.2.2 Velocity (Non-Particulate) Traverses. When velocity or
volumetric flow rate is to be determined (but not particulate
matter) , the same procedure as that used for particulate traverses
(Section 2.2.1) is followed, except that Figure 1-2 may be used
instead of Figure 1-1.
2.3 Cross-Sectional Layout and Location of Traverse Points.
2.3.1 Circular Stacks. Locate the traverse points on two
perpendicular diameters according to Table 1-2 and the example
shown in Figure 1-3. Any equation (for examples, see Citations 2
and 3 in the Bibliography) that gives the same values as those in
Table 1-2 may be used in lieu of Table 1-2.
For particulate traverses, one of the diameters must be in a plane
containing the greatest expected concentration variation, e.g.,
after bends, one diameter shall be in the plane of the bend. This
requirement becomes less critical as the distance from the
disturbance increases; therefore, other diameter locations may be
used, subject to the approval of the Administrator.
In addition, for stacks having diameters greater than 0.61 m (24
in.), no traverse points shall be within 2.5 centimeters (1.00 in.)
of the stack walls; and for stack diameters equal to or less than
0.61 m (24 in.), no traverse points shall be located within 1.3 cm
(0.50 in.) of the stack walls. To meet these criteria, observe the
procedures given below.
2.3.1.1 Stacks With Diameters Greater Than 0.61 m (24 in.). When
any of the traverse points as located in Section 2.3.1 fall within
2.5 cm (1.00 in.) of the
stack walls, relocate them away from the stack walls to: (1) a
distance of
2.5 cm (1.00 in.); or (2) a distance equal to the nozzle inside
diameter, whichever is larger. These relocated traverse points (on
each end of a diameter) shall be the "adjusted" traverse points.
-------
EMTIC TM-001 EMTIC NSPS TEST METHOD Page 4
Whenever two successive traverse points are combined to form a
single adjusted traverse point, treat the adjusted point as two
separate traverse points, both in the sampling (or velocity
measurement) procedure, and in recording the data.
2.3.1.2 Stacks With Diameters Equal To or Less Than 0.61 m (24
in.). Follow the procedure in Section 2.3.1.1, noting only that
any "adjusted" points should be relocated away from the stack walls
to: (1) a distance of 1.3 cm (0.50 in.); or (2) a distance equal to
the nozzle inside diameter, whichever is larger.
2.3.2 Rectangular Stacks. Determine the number of traverse points
as explained in Sections 2.1 and 2.2 of this method. From Table 1-
1, determine the grid configuration. Divide the stack cross-
section into as many equal rectangular elemental areas as traverse
points, and then locate a traverse point at the centroid of each
equal area according to the example in Figure 1-4.
If the tester desires to use more than the minimum number of
traverse points, expand the "minimum number of traverse points"
matrix (see Table 1-1) by adding the extra traverse points along
one or the other or both legs of the matrix; the final matrix need
not be balanced. For example, if a 4 x 3 "minimum number of
points" matrix were expanded to 36 points, the final matrix could
be 9 x 4 or 12 x 3, and would not necessarily have to be 6 x 6.
After constructing the final matrix, divide the stack cross-section
into as many equal rectangular, elemental areas as traverse points,
and locate a traverse point at the centroid of each equal area. The
situation of traverse points being too close to the stack walls is
not expected to arise with rectangular stacks. If this problem
should ever arise, the Administrator must be contacted for
resolution of the matter.
2.4 Verification of Absence of Cyclonic Flow. In most stationary
sources, the direction of stack gas flow is essentially parallel to
the stack walls. However, cyclonic flow may exist (1) after such
devices as cyclones and inertial demisters following venturi
scrubbers, or (2) in stacks having tangential inlets or other duct
configurations which tend to induce swirling; in these instances,
the presence or absence of cyclonic flow at the sampling location
must be determined. The following techniques are acceptable for
this determination. Level and zero the manometer. Connect a Type
S pitot tube to the manometer. Position the Type S pitot tube at
each traverse point, in succession, so that the planes of the face
openings of the pitot tube are perpendicular to the stack cross-
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EMTIC TM-001 EMTIC NSPS TEST METHOD Page 5
sectional plane; when the Type S pitot tube is in this position, it
is at "0° reference." Note the differential pressure (Ap) reading
at each traverse point. If a null (zero) pitot reading is obtained
at 0° reference at a given traverse point, an acceptable flow
condition exists at that point. If the pitot reading is not zero
at 0° reference, rotate the- pitot tube (up to ±90° yaw angle) ,
until a null reading is obtained. Carefully determine and record
the value of the rotation angle (a) to the nearest degree. After
the null technique
has been applied at each traverse point, calculate the average of
the absolute values of a; assign a values of 0° to those points for
which no rotation was required, and include these in the overall
average. If the average value of a is greater than 20°, the
overall flow condition in the stack is unacceptable, and
alternative methodology, subject to the approval of the
Administrator, must be used to perform accurate sample and velocity
traverses. The alternative procedure described in Section 2.5 may
be used to determine the rotation angles in lieu of the procedure
described above.
2.5 Alternative Measurement Site Selection Procedure. This
alternative applies to sources where measurement locations are less
than 2 equivalent or duct diameters downstream or less than one-
half duct diameter upstream from a flow disturbance. The
alternative should be limited to ducts larger than 24 in. in
diameter where blockage and wall effects are minimal. A
directional flow-sensing probe is used to measure pitch and yaw
angles of the gas flow at 40 or more traverse points; the resultant
angle is calculated and compared with acceptable criteria for mean
and standard deviation.
NOTE: Both the pitch and yaw angles are measured from a line
passing through the traverse point and parallel to the stack axis.
The pitch angle is the angle of the gas flow component in the plane
that INCLUDES the traverse line and is parallel to the stack axis.
The yaw angle is the angle of the gas flow component in the plane
PERPENDICULAR to the traverse line at the traverse point and is
measured from the line passing through the traverse point and
parallel to the stack axis.
2.5.1 Apparatus.
2.5.1.1 Directional Probe. Any directional probe, such as United
Sensor Type DA Three-Dimensional Directional Probe, capable of
measuring both the pitch and yaw angles of gas flows is acceptable.
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EMTIC TM-001 EMTIC NSPS TEST METHOD Page 6
(NOTE: Mention of trade name or specific products does not
constitute endorsement by the U.S. Environmental Protection
Agency.) Assign an identification number to the directional probe,
and permanently mark or engrave the number on the body of the
probe. The pressure holes of directional probes are susceptible to
plugging when used in particulate-laden gas streams. Therefore, a
system for cleaning the pressure holes by "back-purging" with
pressurized air is required.
2.5.1.2 Differential Pressure Gauges. Inclined manometers, U-tube
manometers, or other differential pressure gauges (e.g., magnehelic
gauges) that meet the specifications described in Method 2, Section
2.2.
NOTE: If the differential pressure gauge produces both negative
and positive readings, then both negative and positive pressure
readings shall be calibrated at a minimum of three points as
specified in Method 2, Section 2.2.
2.5.2 Traverse Points. Use a minimum of 40 traverse points for
circular ducts and 42 points for rectangular ducts for the gas flow
angle determinations. Follow Section 2.3 and Table 1-1 or 1-2 for
the location and layout of the traverse points. If the measurement
location is determined to be acceptable
according to the criteria in this alternative procedure, use the
same traverse point number and locations for sampling and velocity
measurements.
2.5.3 Measurement Procedure.
2.5.3.1 Prepare the directional probe and differential pressure
gauges as recommended by the manufacturer. Capillary tubing or
surge tanks may be used to dampen pressure fluctuations. It is
recommended, but not required, that a pretest leak check be
conducted. To perform a leak check, pressurize or use suction on
the impact opening until a reading of at least 7.6 cm (3 in.) H20
registers on the differential pressure gauge, then plug the impact
opening. The pressure of a leak-free system will remain stable for
at least 15 seconds.
2.5.3.2 Level and zero the manometers. Since the manometer level
and zero may drift because of vibrations and temperature changes,
periodically check the level and zero during the traverse.
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EMTIC TM-001 EMTIC NSPS TEST METHOD Page 7
2.5.3.3 Position the probe at the appropriate locations in the gas
stream, and rotate until zero deflection is indicated for the yaw
angle pressure gauge. Determine and record the yaw angle. Record
the pressure gauge readings for the pitch angle, and determine the
pitch angle from the calibration curve. Repeat this procedure for
each traverse point. Complete a "back-purge" of the pressure lines
and the impact openings prior to measurements of each traverse
point .
A post-test check as described in Section 2.5.3.1 is required. If
the criteria for a leak-free system are not met, repair the
equipment, and repeat the flow angle measurements.
2.5.4 Calculate the resultant angle at each traverse point, the
average resultant angle, and the standard deviation using the
following equations. Complete the calculations retaining at least
one extra significant figure beyond that of the acquired data.
Round the values after the final calculations.
2.5.4.1 Calculate the resultant angle at each traverse point:
Ri = arc cosine [ (cosineY.J (cosineP..^ ]
Eq. 1-2
Where:
Ri = resultant angle at traverse point i, degree.
Yi = yaw angle at traverse point i, degree.
Pi = pitch angle at traverse point i, degree.
2.5.4.2 Calculate the average resultant for the measurements:
Eq. 1-3
Where:
Ravg = average resultant angle, degree.
n = total number of traverse points.
2.5.4.3 Calculate the standard deviations:
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EMTIC TM-001
EMTIC NSPS TEST METHOD
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E (Ri-
(n-1)
Where:
standard deviation, degree.
2.5.5 The measurement location is acceptable if Ra
<, 10°.
vg
Eg,
20° and S
2.5.6 Calibration. Use a flow system as described in Sections
4.1.2.1 and 4.1.2.2 of Method 2. In addition, the flow system
shall have the capacity to generate two test-section velocities:
one between 365 and 730 m/min (1200 and 2400 ft/min) and one
between 730 and 1100 m/min (2400 and 3600 ft/min) .
2.5.6.1 Cut two entry ports in the test section. The axes through
the entry ports shall be perpendicular to each other and intersect
in the centroid of the test section. The ports should be elongated
slots parallel to the axis of the test section and of sufficient
length to allow measurement of pitch angles while maintaining the
pitot head position at the test-section centroid. To facilitate
alignment of the directional probe during calibration, the test
section should be constructed of plexiglass or some other
transparent material. All calibration measurements should be made
at the same point in the test section, preferably at the centroid
of the test section.
2.5.6.2 To ensure that the gas flow is parallel to the central
axis of the test section, follow the procedure in Section 2.4 for
cyclonic flow determination to measure the gas flow angles at the
centroid of the test section from two test ports located 90° apart.
The gas flow angle measured in each port must be ±2° of 0°.
Straightening vanes should be installed, if necessary, to meet this
criterion.
2.5.6.3 Pitch Angle Calibration. Perform a calibration traverse
according to the manufacturer's recommended protocol in 5°
increments for angles from -60° to +60° at one velocity in each of
the two ranges specified above. Average the pressure ratio values
obtained for each angle in the two flow ranges, and plot a
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EMTIC TM-001 EMTIC NSPS TEST METHOD Page 9
calibration curve with the average values of the pressure ratio (or
other suitable measurement factor as recommended by the
manufacturer) versus the pitch angle. Draw a smooth line through
the data points. Plot also the data values for each traverse
point. Determine the differences between the measured datavalues
and the angle from the calibration curve at the same pressure
ratio. The difference at each comparison must be within 2° for
angles between 0° and 40° and within 3° for angles between 40° and
60°.
2.5.6.4 Yaw Angle Calibration. Mark the three-dimensional probe
to allow the determination of the yaw position of the probe. This
is usually a line extending the length of the probe and aligned
with the impact opening. To determine the accuracy of measurements
of the yaw angle, only the zero or null position need be calibrated
as follows: Place the directional probe in the test section, and
rotate the probe until the zero position is found. With a
protractor or other angle measuring device, measure the angle
indicated by the yaw angle indicator on the three-dimensional
probe. This should be within 2° of 0°. Repeat this measurement
for any other points along the length of the pitot where yaw angle
measurements could be read in order to account for variations in
the pitot markings used to indicate pitot head positions.
BIBLIOGRAPHY
1. Determining Dust Concentration in a Gas Stream, ASME
Performance Test Code No. 27. New York. 1957.
2. DeVorkin, Howard, et al. Air Pollution Source Testing Manual.
Air Pollution Control District. Los Angeles, CA. November
1963.
3. Methods for Determining of Velocity, Volume, Dust and Mist
Content of Gases. Western Precipitation Division of Joy
Manufacturing Co. Los Angeles, CA. Bulletin WP-50. 1968.
4. Standard Method for Sampling Stacks for Particulate Matter.
In: 1971 Book of ASTM Standards, Part 23. ASTM Designation D
2928-71. Philadelphia, PA. 1971.
5. Hanson, H.A., et al. Particulate Sampling Strategies for
Large Power Plants Including Nonuniform Flow. USEPA, ORD,
ESRL, Research Triangle Park, NC. EPA-600/2-76-170. June
-------
EMTIC TM-001
EMTIC NSPS TEST METHOD
Page 10
1976.
6. Entropy Environmentalists, Inc. Determination of the Optimum
Number of Sampling Points: An Analysis of Method 1 Criteria.
Environmental Protection Agency. Research Triangle Park, NC.
EPA Contract No. 68-01-3172, Task 7.
7. Hanson, H.A., R.J. Davini, J.K. Morgan, and A.A. Iversen.
Particulate Sampling Strategies for Large Power Plants
Including Nonuniform Flow. USEPA, Research Triangle Park, NC.
Publication No. EPA-600/2-76-170. June 1976. 350 p.
8. Brooks, E.F., and R.L. Williams. Flow and Gas Sampling
Manual. U.S. Environmental Protection Agency. Research
Triangle Park, NC. Publication No. EPA-600/2-76-203. July
1976. 93 p.
9. Entropy Environmentalists, Inc. Traverse Point Study. EPA
Contract No. 68-02-3172. June 1977. 19 p.
10. Brown, J. and K. Yu. Test Report: Particulate Sampling
Strategy in Circular Ducts. Emission Measurement Branch.
Emission Standards and Engineering Division. U.S.
Environmental Protection Agency, Research Triangle* Park, NC
27711. July 31, 1980. 12 p.
11. Hawksley, P.G.W., S. Badzioch, and J.H. Blackett. Measurement
of Solids in Flue Gases. Leatherhead, England, The British
Coal Utilisation Research Association. 1961. p. 129-133.
12. Knapp, K.T. The Number of Sampling Points Needed for
Representative Source Sampling. In: Proceedings of the Fourth
National Conference on Energy and Environment. Theodore, L.
et al. (ed). Dayton, Dayton Section of the American Institute
of Chemical Engineers. October 3-7, 1976. p. 563-568.
13. Smith, W.S. and D.J. Grove. A Proposed Extension of EPA
Method 1 Criteria. Pollution Engineering. XV (8):36-37.
August 1983.
14. Gerhart, P.M. and M.J. Dorsey. Investigation of Field Test
Procedures for Large Fans. University of Akron. Akron, OH.
(EPRI Contract'CS-1651). Final Report (RP-1649-5) . December
1980.
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EMTIC TM-001 EMTIC NSPS TEST METHOD Page 11
15. Smith, W.S. and D.J. Grove. A New Look at Isokinetic Sampling
Theory and Applications. Source Evaluation Society
Newsletter. VIII(3):19-24. August 1983.
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EMTIC TM-001
EMTIC NSPS TEST METHOD
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Table 1-1. CROSS-SECTION LAYOUT FOR
RECTANGULAR STACKS
Matrix layout
-Number of traverse points
9
12
16
20
25
30
36
42
49
3x3
4x3
4x4
5x4
5x5
, 6x5
, 6x6
, 7x6
7x7
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EMTIC TM-001
EMTIC NSPS TEST METHOD
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TABLE 1-2
LOCATION OF TRAVERSE POINTS IN CIRCULAR STACKS
(Percent of stack diameter from inside
wall to traverse point)
Traverse
Point
Number on a
Diameter
1
2
3
4
5
6
7
8
9
10 ....
11 ....
12 ....
13 ....
Number of traverse points on a diameter
2
14
.6
85
.4
4
6.
7
25
.0
75
.0
93
.3
6
4.
4
14
.6
29
.6
70
.4
85
.4
95
.6
8
3.
2
10
.5
19
.4
32
.3
67
.7
80
.6
89
.5
96
.8
10
2.6
8.2
14.
6
22.
6
34.
2
65.
8
77.
4
85.
4
91.
8
97.
4
12
2.1
6.7
11.
8
17.
7
25.
0
35.
6
64.
4
75.
0
82.
3
88.
2
93.
3
97.
9
14
1.8
5.7
9.9
14.
6
20.
1
26.
9
36.
6
63.
4
73.
1
79.
9
85.
4
90.
1
94.
3
16
1.6
4. 9
8.5
12.
5
16.
9
22.
0
28.
3
37.
5
62.
5
71.
7
78.
0
83.
1
87.
5
18
1.
4
4.
4
7.
5
10
.9
14
.6
18
.8
23
.6
29
.6
38
.2
61
.8
70
.4
76
.4
81
.2
20
1.
3
3.
9
6.
7
9.
7
11
2.
9
16
.5
20
.4
25
.0
30
.6
38
.8
61
.2
69
.4
75
.0
22
1.1
3.5
6.0
8.7
11.
6
14.
6
18.
0
21.
8
26.
2
31.
5
39.
3
60.
7
68.
5
24
1.1
3.2
5.5
7.9
10.
5
13.
2
16.
1
19.
4
23.
0
27.
2
32.
3
39.
8
60.
2
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EMTIC TM-001
EMTIC NSPS TEST METHOD
Page 14
14 ....
15 ....
16 ....
17 ....
18 ....
19 ....
20 ....
21 ....
22 ....
23 ....
24 ....
98.
2
91.
5
95.
1
98.
4
85
.4
89
.1
92
.5
95
.6
98
.6
79
.6
83
.5
87
.1
90
.3
93
.3
96
.1
98
.7
73.
8
78.
2
82.
0
85.
4
"88.
4
91.
3
94.
0
96.
5
98.
9
67.
7
72.
8
77.
0
80.
6
83.
9
86.
8
89.
5
92.
1
94.
5
96.
8
98.
9
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EMTIC TM-001
EMTIC NSPS TEST METHOD
Page 15
0.5
Duct Diameters Upstream from Row Disturbance* (Distance A)
1.0 1.5 2.0
2.5
40
30
10
0
I I I
*High«r Numbtr i« lor
Rectangular Stacks or Dud*
24 or 25
- 'From Point ol Any Type of
I
20
I
16
I
V. ^Disturbance
-1"
r
B
Maaiuramant
|_ Sita
Disturbance
V^=1
-
—
Stack Oiamatar > 0.61 m (24 in.)
12
.or.'
Disturbance (Bend, Expansion. Contraction, ate.)
Stack Diameter- 0.30 to 081 m (12-24 in.)
I I I
345678
Duct Diameters Downstream from Flow Disturbance* (Distance B)
10
Figure 1-1. Minimum number of traverse points for
particulate traverses.
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EMTIC TM-001
EMTIC NSPS TEST METHOD
Page 16
so
0.5
40 -
30 -
10 -
Duct Diameters Upstream from Flow Disturbance* (Distance A)
1.0 1.5 2.0
2.5
I I I I I I
" Higher Number is for
Rectangular Stacks or Ducts
I
I
7
B
I
^xuistuitanee
Measurement
[_ Sit*
~"
Disturbance
V — I
-
1 6 stack Diameter > 0.61 m (24 in.)
~~ |
— * From Point of Any Type of
Disturbance (Bend, Expansion. Contraction, etc.)
12
8or98 -
Stack Diameter » 0.30 to 0.61 m (12-24 in.)
I I I I I I
I
345678
Duct Diameters Downstream from Flow Disturbance* (Distance B)
10
Figure 1-2. Minimum number of traverse points for velocity
(nonparticulate) traverses.
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EMTIC TM-001
EMTIC NSPS TEST METHOD
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Traverse
Pant
1
2
3
4
5
6
Distance
%o( diameter
4.4
147
2S.5
70.5
85.3
95.6
Figure 1-3. Example showing circular stack cross section
divided into 12 equal areas, with location of traverse
points indicated.
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EMTIC TM-001
EMTIC NSPS TEST METHOD
Page 18
0
o
0
o
o
0
o
o
1
o
o
o
0
Figure 1-4. Example showing rectangular stack cross section
divided into 12 equal areas, with a traverse point at centroid
of each area.
-------
STACK SAMPLING CYCLONIC FLOW
General
Conventional sampling procedures are not applicable to stacks with
cyclonic flow due to the presence of non-axial flow components. This
appendix describes a method for sampling stacks with cyclonic flow; I.e.
flow with tangential velocity components. Cyclonic flow may exist after
cyclones, tangential Inlets, or other configurations that may tend to
Induce swirling.
Several different approaches have been devised to minimize the biasing
effects of non-axial flow. The method discussed In this appendix
utilizes the alignment approach to reduce or eliminate the bias produced
by misalignment of the sampling nozzle and pltot tubes with the path of
the particles. Sampling results obtained with this method must be
reviewed for possible Inherent bias (see section entitled Accuracy
Considerations) to determine acceptability for any purpose.
Accuracy Considerations
As discussed 1n Chapter 5, small (light) particles tend to follow the
flow stream while Jarge (heavy) particles tend to be affected more by
their own Inertia than by the flow stream. Due to the effects of the
cyclonic condition and centrifugal action, components of radial velocity
should be Imparted to large particles, while small particles continue to
follow the flow stream. If the sampling ports are sufficiently down-
stream of the onset of cyclonic flow (at least two stack diameters),
large particles should have moved to the vicinity of the stack wall and
no longer have radial velocity components. For this reason, this method
does not consider components of radial velocity, and the term 'total
velocity vector' refers to the resultant of the vertical (parallel to
the stack axis) velocity vector and the tangential velocity vector.
Although sampling by the alignment approach Is done In the direction of
flow of the stack gas at each sample point, bias may still be produced
If the path of the particles 1s not 1n the direction of flow. Small
particles follow the flow stream and large particles at the stack will
have no radial velocity components so the only source of bias should be
large particles near the stack wall that may not be moving In the direc-
tion of flow, I.e. unequal tangential velocity components. An Indica-
tion of the distribution of large and small particles may be obtained by
comparing the probe wash and cyclone catch to the filter and Implnger
catch. Large particles that do not follow the flow stream should be
caught In the probe and cyclone, while small particles should be caught
on the filter and In the 1mp1ngers. Such comparison may yield
-------
Information on possible bias 1n the sample since bias 1s produced by
large particles, but should not be considered to be an accurate deter-
mination of particle size distribution. If the large particles Mere not
moving In the direction of flow In the stack, the large/small particle
proportion In the sampling train may not be the same as In the stack.
If all particles are Moving parallel to the direction of flow* no bits
should be produced.
If the pollutant 1s or behaves as a gas, no bias 1s produced by par-
ticles novlng 1n directions other than parallel to the flow strew.
This method provides an accurate determination of velocity and flow
rate, which are requirements of gaseous sampling (Chapter 6)* The
larger the proportion of the total catch that behaves as a gas (filter
and Inplngers), the greater the confidence In the sample being without
bias.
Determining Cyclonic Flow •
The existence of cyIconic flow Is determined by measuring the flow angle
at each sample point. The flow angle 1s the angle between the direction
of flow and the axis of the stack. If the average of the absolute val-
ues of the flow angles 1s greater than 20*, cyclonic flow exists to such
an extent that special sampling procedures are necessary.
The direction of flow Is determined by locating the pltot tube null posi-
tion at each sample point. The pltot tube null position at a sample
point 1s determined by rotating the pltot tubes around the axis of the
probe until a zero manometer reading Is obtained. Advance knowledge of
the direction of the tangential flow component Is helpful for the Ini-
tial rotation of the pltot tubes since the plane through the pltot tubes
must be perpendicular to the total velocity vector to obtain a null read-
Ing on the manometer. The angle between the plane through the pltot
tubes 1n the null position and the stack cross^sectional pTane Is equal
In magnitude to the flow angle; the magnitude of the angle may be
measured with the pltot tubes In the null position or after the pltot
tubes have been rotated 90* Into the flow stream for velocity measure-
ment. A magnetic protractor-level Is a convenient angle Measuring de-
vice; scribe marks on the sample box with a pointer on the probe (or
vice-versa) may be satisfactory If proper alignment with the axis of the
stack and the plane of the pltot tubes Is maintained.
In some cases of cyclonic flow, the flow angle may be greater than 90*
at some sample points, Indicating flow back Into the stack at those
particular sample points. If the now angle 1s greater than 90*, It 1s
recorded as 90* so that sample points with negative velocity are con-
sidered to have no vertical velocity (cos 90* • 0). The existence of
sample points with negative velocity nay be determined with the pltot
tubes aligned with the flow stream; the manometer deflection will Indi-
cate the direction of flow.
-------
Sampling Procedure
•»__•!«__••& ^_^__^__ f
Standard 1sok1net1c sampling procedures (Chapters 4 and 5) are foil owed
except for adjustment of the sampling tine and pi tot tube and nozzle
orientation at each sample point.
Preliminary Velocity Traverse and Calculations
Knowledge of the flow angles at all sampling points Is necessary to
Insure that the total sample time and total sample volume Is adequate; •
therefore, flow angles are normally measured during the preliminary
velocity traverse. The complete set of angles should be measured In as
short a duration of time as possible 1n case the position of the flow
cyclone In the stack Is changing with time. After the measurement of
flow angles Is complete, a base sampling time for each sampling point Is
selected. The actual sampling time at each sample point Is the base
sampling time multiplied by the cosine of the flow angle at that sample
point.
All preliminary procedures and calculations are performed with prelimi-
nary data as measured 1n the direction of flow similar to standard 1 so-
kinetic sampling procedures. The actual sampling time at each sample
point (base time x cos a) Is used In preliminary calculations. As
discussed earlier, 1f zero or negative flow exists at any sample point,
the flow angle 1s recorded as 9
-------
periods between sample points, but the off-time oust not be so long that
the sample could be contaminated by particles entering the sampling
train while the flow 1s stopped.
In some cases of cyclonic flow, some sample points may have negative
flow or flow back Into the stack (flow angle > 9(f) rather than out the
stack. These sampling points are treated as points with zero flow and
zero actual sampling time. This situation may cause the results to be
biased high If some of the pollutant sampled at the sample points with
positive flow Is also present at the sample points with negative flow.
Two separate samples may produce more accurate results 1n such a cast -
one sample for positive flow and one sample for negative flow with the
numerical difference being the emission rate.
The field check of percent 1sok1net1c Is made using actual parameters
measured during sampling; velocity Is used as measured 1n the flow
stream and time Is the sum of the adjusted (actual) sampling times for
the separate sample points. -The Isoklnetlc check could also be per-
formed by calculating the vertical velocity component at each sample
point and using the total base time as explained In the section on Data
Reduction, but this approach 1s considered too cumbersome for field use.
Data Reduction
Data reduction procedures must account for the differences between the
total velocity vectors (defined by a and AP) and the exiting components
of these vectors. Since the average exiting velocity oust be used to
calculate stack flow rate (ACFM or SCFN), effective stack height, and.
1n turn, allowable emission rate and standard effective stack height,
data reduction procedures must average only the vertical components of
the total velocity vectors. Different data reduction approaches may
yield correct results; the data reduction procedures discussed In this
section are based on adjustment of Individual AP readings to correspond
to vertical velocity components. Standard data reduction procedures are
discussed 1n Chapter 8 and only the adjustments to the Input data neces-
sary to apply the standard procedures are discussed here.
Each fleldAP reading (as measured In the flow stream) 1s multiplied by
the square of the cosine of the flow angle (a) corresponding to each AP
reading. Data reduction Input AP 1s (cos2 a) (fleldAP). Input sample
time per sample point Is the total base sampling time per sample point
and the total sampling time Input Is the total base time (base time)
(number of sample points). All other parameters are Input as measured.
The data sheets In Appendix D should be helpful 1n organizing cyclonic
flow data.
-------
CYCLONIC FLOW FIELD CALCULATION SHEET
Company Name
Address
Date
Sampling Location
T««c Tin* - co» * (BM« Tina)
Tester
Base Test: Tina
Sample
Point
•
.
tagle
*
Time
•
Ron t
•
&P
cos*(VEp)
.
*
I
'
Bon 1 .
AP
.
cos* (£P)
Run t
*P
co«4(VSp)
•
Averagt
Averagt Apy
Averagt &P,
-------
Appendix G.2
EPA Method 2
-------
EMISSION MEASUREMENT TECHNICAL INFORMATION CENTER
NSPS TEST METHOD
Method 2 - Determination of Stack Gas Velocity and Volumetric
Flow Rate (Type S Pitot Tube)
1. PRINCIPLE AND APPLICABILITY
1.1 Principle. The average gas velocity in a stack is determined from the gas
density and from measurement of the average velocity head with a Type S
(Stausscheibe or reverse type) pitot tube.
1.2 Applicability. This method is applicable for measurement of the average
velocity of a gas stream and for quantifying gas flow.
This procedure is not applicable at measurement sites that fail to meet the
criteria of Method 1, Section 2.1. Also, the method cannot be used for direct
measurement in cyclonic or swirling gas streams; Section 2.4 of Method 1 shows
how to determine cyclonic or swirling flow conditions. When unacceptable
conditions exist, alternative procedures, subject to the approval of the
Administrator, U.S. Environmental Protection Agency, must be employed to make
accurate flow rate determinations; examples of such alternative procedures are:
(1) to install straightening vanes; (2) to calculate the total volumetric flow
rate stoichiometrically, or (3) to move to another measurement site at which the
flow is acceptable.
2. APPARATUS
Specifications for the apparatus are given below. Any other apparatus that has
been demonstrated (subject to approval of the Administrator) to be capable of
meeting the specifications will be considered acceptable.
2.1 Type S Pitot Tube. Pitot tube made of metal tubing (e.g., stainless steel)
as shown in Figure 2-1. It is recommended that the external tubing diameter
(dimension Dt, Figure 2-2b) be between 0.48 and 0.95 cm (3/16 and 3/8 inch).
There shall be an equal distance from the base of each leg of the pitot tube to
its face-opening plane (dimensions PA and ft, Figure 2-2b); it is recommended
that this distance be between 1.05 and 1.50 times the external tubing diameter.
The face openings of the pitot tube shall, preferably, be aligned as shown in
Figure 2-2; however, slight misalignments of the openings are permissible (see
Figure 2-3) .
The Type S pitot tube shall have a known coefficient, determined as outlined in
Section 4. An identification number shall be assigned to the pitot tube; this
Prepared by Emission Measurement Branch EMTIC M-002
Technical Support Division, OAQPS, EPA
-------
EMISSION MEASUREMENT TECHNICAL INFORMATION CENTER
NSPS TEST METHOD
number shall be permanently marked or engraved on the body of the tube. A
standard pitot tube may be used instead of a Type S, provided that it meets the
specifications of Sections 2.7 and 4.2; note, however, that the static and impact
pressure holes of standard pitot tubes are susceptible to plugging in
particulate-laden gas streams. Therefore, whenever a standard pitot tube is used
to perform a traverse, adequate proof must be furnished that the openings of the
pitot tube have not plugged up during the traverse period; this can be done by
taking a velocity head (Ap) reading at the final traverse point, cleaning out the
impact and static holes of the standard pitot tube by "back-purging" with
pressurized air, and then taking another Ap reading. If the Ap readings made
before and after the air purge are the same (±5 percent) , the traverse is
acceptable. Otherwise, reject the run. Note that if Ap at the final traverse
point is unsuitably low, another point may be selected. If "back-purging" at
regular intervals is part of the procedure, then comparative Ap readings shall
be taken, as above, for the last two back purges at which suitably high Ap
readings are observed.
2.2 Differential Pressure Gauge. An inclined manometer or equivalent device.
Most sampling trains are equipped with a 10-in. (water column) inclined-vertical
manometer, having 0.01-in. H2O divisions on the 0- to 1-in. inclined scale, and
0.1-in. H20 divisions on the 1- to 10-in. vertical scale. This type of manometer
(or other gauge of equivalent sensitivity) is satisfactory for the measurement
of Ap values as low as 1.3 mm (0.05 in.) H20. However, a differential pressure
gauge of greater sensitivity shall be used (subject to the approval of the
Administrator) , if any of the following is found to be true: (1) the arithmetic
average of all Ap readings at the traverse points in the stack is less than
1.3 mm (0.05 in.) H20; (2) for traverses of 12 or more points, more than 10
percent of the individual Ap readings are below 1.3 mm (0.05 in.) H20; (3) for
traverses of fewer than 12 points, more than one Ap reading is below 1.3 mm
(0.05 in.) H20. Citation 18 in the Bibliography describes commercially available
instrumentation for the measurement of low-range gas velocities.
As an alternative to criteria (1) through (3) above, the following calculation
may be performed to determine the necessity of using a more sensitive
differential pressure gauge:
Prepared by Emission Measurement Branch EMTIC M-002
Technical Support Division, OAQPS, EPA
-------
EMTIC TM-002
NSPS TEST METHOD
Page 3
Where:
T =
1=1
n
K
Individual velocity head reading at a traverse point, mm (in.)
H20.
Total number of traverse points.
0.13 mm H20 when metric units are used and 0.005 in. H20 when
English units are used.
If T is greater than 1.05, the velocity head data are unacceptable and a more
sensitive differential pressure gauge must be used.
NOTE: If differential pressure gauges other than inclined manometers are used
(e.g., magnehelic gauges), their calibration must be checked after each test
series. To check the calibration of a differential pressure gauge, compare Ap
readings of the gauge with those of a gauge-oil manometer at a minimum of three
points, approximately representing the range of Ap values in the stack. If, at
each point, the values of Ap as read by the differential pressure gauge and
gauge-oil manometer agree to within 5 percent, the differential pressure gauge
shall be considered to be in proper calibration. Otherwise, the test series
shall either be voided, or procedures to adjust the measured Ap values and final
results shall be used, subject to the approval of the Administrator.
2.3 Temperature Gauge. A thermocouple, liquid-filled bulb thermometer,
bimetallic thermometer, mercury-in-glass thermometer, or other gauge capable of
measuring temperature to within 1.5 percent of the minimum absolute stack
temperature. The temperature gauge shall be attached to the pitot tube such that
the sensor tip does not touch any metal; the gauge shall be in an interference-
free arrangement with respect to the pitot tube face openings (see Figure 2-1 and
also Figure 2-7 in Section 4). Alternative positions may be used if the pitot
tube-temperature gauge system is calibrated according to the procedure of Section
4. Provided that a difference of not more than 1 percent in the average velocity
measurement is introduced, the temperature gauge need not be attached to the
pitot tube; this alternative is subject to the approval of the Administrator.
2.4 Pressure Probe and Gauge. A piezometer tube and mercury- or water-filled
U-tube manometer capable of measuring stack pressure to within 2.5 mm (0.1 in.)
Hg. The static tap of a standard type pitot tube or one leg of a Type S pitot
tube with the face opening planes positioned parallel to the gas flow may also
be used as the pressure probe.
-------
EMTIC TM-002 NSPS TEST METHOD Page 4
2.5 Barometer. A mercury, aneroid, or other barometer capable of measuring
atmospheric pressure to within 2.5 mm (0.1 in.) Hg. See NOTE in Method 5,
Section 2.1.9.
2.6 Gas Density Determination Equipment. Method 3 equipment, if needed (see
Section 3.6), to determine the stack gas dry molecular weight, and Reference
Method 4 or Method 5 equipment for moisture content determination; other methods
may be used subject to approval of the Administrator.
2.7 Calibration Pitot Tube. When calibration of the Type S pitot tube is
necessary (see Section 4) , a standard pitot tube for a reference. The standard
pitot tube shall, preferably, have a known coefficient, obtained either (1)
directly from the National Bureau of Standards, Route 70 S, Quince Orchard Road,
Gaithersburg, Maryland, or (2) by calibration against another standard pitot tube
with an NBS-traceable coefficient. Alternatively, a standard pitot tube designed
according to the criteria given in Sections 2.7.1 through 2.7.5 below and
illustrated in Figure 2-4 (see also Citations 7, 8, and 17 in the Bibliography)
may be used. Pitot tubes designed according to these specifications will have
baseline coefficients of about 0.99 ± 0.01.
2.7.1 Hemispherical (shown in Figure 2-4) ellipsoidal, or conical tip.
2.7.2 A minimum of six diameters straight run (based upon D, the external
diameter of the tube) between the tip and the static pressure holes.
2.7.3 A minimum of eight diameters straight run between the static pressure
holes and the centerline of the external tube, following the 90-degree bend.
2.7.4 Static pressure holes of equal size (approximately 0.1 D), equally spaced
in a piezometer ring configuration.
2.7.5 Ninety-degree bend, with curved or mitered junction.
2.8 Differential Pressure Gauge for Type S Pitot Tube Calibration. An inclined
manometer or equivalent. If the single-velocity calibration technique is
employed (see Section 4.1.2.3), the calibration differential pressure gauge shall
be readable to the nearest 0.13 mm (0.005 in.) H20. For multivelocity
calibrations, the gauge shall be readable to the nearest 0.13 mm (0.005 in.) H20
for Ap values between 1.3 and 25 mm (0.05 and 1.0 in.) H20, and to the nearest
1.3 mm (0.05 in.) H20 for Ap values above 25 mm (1.0 in.) H20. A special, more
sensitive gauge will be required to read Ap values below 1.3 mm (0.05 in.) H20
(see Citation 18 in the Bibliography).
3. PROCEDURE
3.1 Set up the apparatus as shown in Figure 2-1. Capillary tubing or surge
tanks installed between the manometer and pitot tube may be used to dampen Ap
fluctuations. It is recommended, but not required, that a pretest leak-check be
conducted as follows: (1) blow through the pitot impact opening until at least
-------
EMTIC TM-002 NSPS TEST METHOD Page 5
7.6 cm (3 in.) H20 velocity pressure registers on the manometer; then, close off
the impact opening. The pressure shall remain stable for at least 15 seconds;
(2) do the same for the static pressure side, except using suction to obtain the
minimum of 7.6 cm (3 in.) H20. Other leak-check procedures, subject to the
approval of the Administrator, may be used.
3.2 Level and zero the manometer. Because the manometer level and zero may
drift due to vibrations and temperature changes, make periodic checks during the
traverse. Record all necessary data as shown in the example data sheet
(Figure 2-5) ,
3.3 Measure the velocity head and temperature at the traverse points specified
by Method 1. Ensure that the proper differential pressure gauge is being used
for the range of Ap values encountered (see Section 2.2). If it is necessary to
change to a more sensitive gauge, do so, and remeasure the Ap and temperature
readings at each traverse point. Conduct a post-test leak-check (mandatory), as
described in Section 3.1 above, to validate the traverse run.
3.4 Measure the static pressure in the stack. One reading is usually adequate.
3.5 Determine the atmospheric pressure.
3.6 Determine the stack gas dry molecular weight. For combustion processes or
processes that emit essentially C02, 02, CO, and N2, use Method 3. For processes
emitting essentially air, an analysis need not be conducted; use a dry molecular
weight of 29.0. For other processes, other methods, subject to the approval of
the Administrator, must be used.
3.7 Obtain the moisture content from Reference Method 4 (or equivalent) or from
Method 5.
3.8 Determine the cross-sectional area of the stack or duct at the sampling
location. Whenever possible, physically measure the stack dimensions rather than
using blueprints.
4. CALIBRATION
4.1 Type S Pitot Tube. Before its initial use, carefully examine the Type S
pitot tube in top, side, and end views to verify that, the face openings of the
tube are aligned within the specifications illustrated in Figure 2-2 or 2-3. The
pitot tube shall not be used if it fails to meet these alignment specifications.
After verifying the face opening alignment, measure and record the following
dimensions of the pitot tube: (a) the external tubing diameter (dimension Dt,
Figure 2-2b) ; and (b) the base-to-opening plane distances (dimensions PA and PB,
Figure 2-2b). If Dt is between 0.48 and 0.95 cm (3/16 and 3/8 in.), and if ft
and PB are equal and between 1.05 and 1.50 Dt, there are two possible options:
(1) the pitot tube may be calibrated according to the procedure outlined in
Sections 4.1.2 through 4.1.5 below, or (2) a baseline (isolated tube) coefficient
value of 0.84 may be assigned to the pitot tube. Note, however, that if the
-------
EMTIC TM-002 NSPS TBST METHOD Page 6
pitot tube is part of an assembly, calibration may still be required, despite
knowledge of the baseline coefficient value (see Section 4.1.1) .
If Dt, ?i , and 8 are outside the specified limits, the pitot tube must be
calibrated as outlined in Sections 4.1.2 through 4.1.5 below.
4.1.1 Type S Pitot Tube Assemblies. During sample and velocity traverses, the
isolated Type S pitot tube is not always used; in many instances, the pitot tube
is used in combination with other source -sampling components (thermocouple,
sampling probe, nozzle) as part of an "assembly." The presence of other sampling
components can sometimes affect the baseline value of the Type S pitot tube
coefficient (Citation 9 in the Bibliography) ; therefore an assigned (or otherwise
known) baseline coefficient value may or may not be valid for a given assembly.
The baseline and assembly coefficient values will be identical only when the
relative placement of the components in the assembly is such that aerodynamic
interference effects are eliminated. Figures 2-6 through 2-8 illustrate
interference -free component arrangements for Type S pitot tubes having external
tubing diameters between 0.48 and 0.95 cm (3/16 and 3/8 in.). Type S pitot tube
assemblies that fail to meet any or all of the specifications of Figures 2-6
through 2-8 shall be calibrated according to the procedure outlined in Sections
4.1.2 through 4.1.5 below, and prior to calibration, the values of the
intercomponent spacings (pitot-nozzle, pitot-thermocouple, pitot-probe sheath)
shall be measured and recorded.
NOTE: Do not use any Type S pitot tube assembly which is constructed such that
the impact pressure opening plane of the pitot tube is below the entry plane of
the nozzle (see Figure 2-6B) .
4.1.2 Calibration Setup. If the Type S pitot tube is to be calibrated, one leg
of the tube shall be permanently marked A, and the other, B. Calibration shall
be done in a flow system having the following essential design features:
4.1.2.1 The flowing gas stream must be confined to a duct of definite cross-
sectional area, either circular or rectangular. For circular cross sections, the
minimum duct diameter shall be 30.5 cm (12 in.); for rectangular cross sections,
the width (shorter side) shall be at least 25.4 cm (10 in.).
*
4.1.2.2 The cross -sectional area of the calibration duct must be constant over
a distance of 10 or more duct diameters. For a rectangular cross section, use
an equivalent diameter, calculated from the following equation, to determine the
number of duct diameters :
D -
(L + W)
Eq. 2-1
where:
-------
EMTIC TM-002 NSPS TEST METHOD Page 7
De = Equivalent diameter.
L = Length.
W = Width.
To ensure the presence of stable, fully developed flow patterns at the
calibration site, or "test section," the site must be located at least eight
diameters downstream and two diameters upstream from the nearest disturbances.
NOTE: The eight- and two-diameter criteria are not absolute; other test section
locations may be used (subject to approval of the Administrator) , provided that
the flow at the test site is stable and demonstrably parallel to the duct axis.
4.1.2.3 The flow system shall have the capacity to generate a test-section
velocity around 915 m/min (3,000 ft/min). This velocity must be constant with
time to guarantee steady flow during calibration. Note that Type S pitot tube
coefficients obtained by single-velocity calibration at 915 m/min (3,000 ft/min)
will generally be valid to ±3 percent for the measurement of velocities above 305
m/min (1,000 ft/min) and to ±5 to 6 percent for the measurement of velocities
between 180 and 305 m/min (600 and 1,000 ft/min) . If a more precise correlation
between Cp and velocity is desired, the flow system shall have the capacity to
generate at least four distinct, time-invariant test-section velocities covering
the velocity range from 180 to 1,525 m/min (600 to 5,000 ft/min), and calibration
data shall be taken at regular velocity intervals over this range (see Citations
9 and 14 in the Bibliography for details).
4.1.2.4 Two entry ports, one each for the standard and Type S pitot tubes, shall
be cut in the test section; the standard pitot entry port shall be located
slightly downstream of the Type S port, so that the standard and Type S impact
openings will lie in the same cross-sectional plane during calibration. To
facilitate alignment of the pitot tubes during calibration, it is advisable that
the test section be constructed of plexiglas or some other transparent material.
4.1.3 Calibration Procedure. Note that this procedure is a general one and must
not be used without first referring to the special considerations presented in
Section 4.1.5. Note also that this procedure applies only to single-velocity
calibration. To obtain calibration data for the A and B sides of the Type S
pitot tube, proceed as follows:
4.1.3.1 Make sure that the manometer is properly filled and that the oil is free
from contamination and is of the proper density. Inspect and leak-check all
pitot lines; repair or replace if necessary.
4.1.3.2 Level and zero the manometer. Turn on the fan, and allow the flow to
stabilize. Seal the Type S entry port.
4.1.3.3 Ensure that the manometer is level and zeroed. Position the standard
pitot tube at the calibration point (determined as outlined in Section 4.1.5.1),
and align the tube so that its tip is pointed directly into the flow. Particular
care should be taken in aligning the tube to avoid yaw and pitch angles. Make
sure that the entry port surrounding the tube is properly sealed.
-------
EMTIC TM-002 NSPS TEST METHOD Page 8
4.1.3.4 Read Apscd, and record its value in a data table similar to the one shown
in Figure 2-9. Remove the standard pitot tube from the duct, and disconnect it
from the manometer. Seal the standard entry port.
4.1.3.5 Connect the Type S pitot tube to the manometer. Open the Type S entry
port. Check the manometer level and zero. Insert and align the Type S pitot
tube so that its A side impact opening is at the same point as was the standard
pitot tube and is pointed directly into the flow. Make sure that the entry port
surrounding the tube is properly sealed.
4.1.3.6 Read Aps, and enter its value in the data table. Remove the Type S
pitot tube from the duct, and disconnect it from the manometer.
4.1.3.7 Repeat Steps 4.1.3.3 through 4.1.3.6 above until three pairs of Ap
readings have been obtained.
4.1.3.8 Repeat Steps 4.1.3.3 through 4.1.3.7 above for the B side of the Type
S pitot tube.
4.1.3.9 Perform calculations, as described in Section 4.1.4 below.
4.1.4 Calculations.
4.1.4.1 For each of the six pairs of Ap readings (i.e., three from side A and
three from side B) obtained in Section 4.1.3 above, calculate the value of
the Type S pitot tube coefficient as follows:
c -c
•~ ^p(std)
Bq. 2-2
Where:
Cp(s) = Type s pitot tube coefficient.
Cpistai = Standard pitot tube coefficient; use 0.99 if the
coefficient is unknown and the tube is designed according
to the criteria of Sections 2.7.1 to 2.7.5 of this
method.
APsta = Velocity head measured by the standard pitot tube, cm
(in.) H20.
Aps = Velocity head measured by the Type S pitot tube, cm (in.)
H20.
4.1.4.2 Calculate Cp (side A), the mean A-side coefficient, and Cp (side B) , the
-------
EMTIC TM-002 NSPS TEST METHOD Page 9
mean B-side coefficient; calculate the difference between these two average
values.
4.1.4.3 Calculate the deviation of each of the three A-side values of
Cp(B) from Cp (side A) , and the deviation of each B-side values of Cp(s, from
Cp (side B). Use the following equation:
Deviation = C ~C_(A or B)
P(s) P
Eq. 2-3
4.1.4.4 Calculate a, the average deviation from the mean, for both the A and B
sides of the pitot tube. Use the following equation:
a(side A or B) =
Eq. 2-4
4.1.4.5 Use the Type S pitot tube only if the values of a (side A) and a (side
B) are less than or equal to 0.01 and if the absolute value of the difference
between Cp (A) and Cp (B) is 0.01 or less.
4.1.5 Special Considerations.
4.1.5.1 Selection of Calibration Point.
4.1.5.1.1 When an isolated Type S pitot tube is calibrated, select a calibration
point at or near the center of the duct, and follow the procedures outlined in
Sections 4.1.3 and 4.1.4 above. The Type S pitot coefficients so obtained,
i.e., Cp (side A) and £ (side B) , will be valid, so long as either: (1) the
isolated pitot tube is used; or (2) the pitot tube is used with other components
(nozzle, thermocouple, sample probe) in an arrangement that is free from
aerodynamic interference effects (see Figures 2-6 through 2-8).
4.1.5.1.2 For Type S pitot tube-thermocouple combinations (without sample
probe), select a calibration point at or near the center of the duct, and follow
the procedures outlined in Sections 4.1.3 and 4.1.4 above. The coefficients so
obtained will be valid so long as the pitot tube-thermocouple combination is used
by itself or with other components in an interference-free arrangement (Figures
2-6 and 2-8) .
4.1.5.1.3 For assemblies with sample probes, the calibration point should be
-------
EMTIC TM-002 NSPS TEST METHOD . Page 10
located at or near the center of the duct; however, insertion of a probe sheath
into a small duct may cause significant cross-sectional area blockage and yield
incorrect coefficient values (Citation 9 in the Bibliography). Therefore, to
minimize the blockage effect, the calibration point may be a few inches off-
center if necessary. The actual blockage effect will be negligible when the
theoretical blockage, as determined by a projected-area model of the probe
sheath, is 2 percent or less of the duct cross-sectional area for assemblies
without external sheaths (Figure 2-10a), and 3 percent or less for assemblies
with external sheaths (Figure 2-10b).
4.1.5.2 For those probe assemblies in which pitot tube-nozzle interference is
a factor (i.e., those in which the pitot-nozzle separation distance fails to meet
the specification illustrated in Figure 2-6A) , the value of Cp(s) depends upon the
amount of free-space between the tube and nozzle, and therefore is a function of
nozzle size. In these instances, separate calibrations shall be performed with
each of the commonly used nozzle sizes in place. Note that the single-velocity
calibration technique is acceptable for this purpose, even though the larger
nozzle sizes (>0.635 cm or 1/4 in.) are not ordinarily used for isokinetic
sampling at velocities around 915 m/min (3,000 ft/min), which is the calibration
velocity; note also that it is not necessary to draw an isokinetic sample during
calibration (see Citation 19 in the Bibliography).
4.1.5.3 For a probe assembly constructed such that its pitot tube is always used
in the same orientation, only one side of the pitot tube need be calibrated (the
side which will face the flow) . The pitot tube must still meet the alignment
specifications of Figure 2-2 or 2-3, however, and must have an average deviation
(a) value of 0.01 or less (see Section 4.1.4.4.)
4.1.6 Field Use and Recalibration.
4.1.6.1 Field Use.
4.1.6.1.1 When a Type S pitot tube (isolated or in an assembly) is used in the
field, the appropriate coefficient value (whether assigned or obtained by
calibration) shall be used to perform velocity calculations. For calibrated Type
S pitot tubes, the A side coefficient shall be used when the A side of the tube
faces the flow, and the B side coefficient shall be used when the B side faces
the flow; alternatively, the arithmetic average of the A and B side coefficient
values may be used, irrespective of which side faces the flow.
4.1.6.1.2 When a probe assembly is used to sample a small duct, 30.5 to 91.4 cm
(12 to 36 in.) in diameter, the probe sheath sometimes blocks a significant part
of the duct cross-section, causing a reduction in the effective value of Cp(8).
Consult Citation 9 in the Bibliography for details. Conventional pitot-sampling
probe assemblies are not recommended for use in ducts having inside diameters
smaller than 30.5 cm (12 in.) (see Citation 16 in the Bibliography) .
4.1.6.2 Recalibration.
4.1.6.2.1 Isolated Pitot Tubes. After each field use, the pitot tube shall be
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EMTIC TM-002 N8PS TEST METHOD Page 11
carefully reexamined in top, side, and end views. If the pitot face openings are
still aligned within the specifications illustrated in Figure 2-2 or 2-3, it can
be assumed that the baseline coefficient of the pitot tube has not changed. If,
however, the tube has been damaged to the extent that it no longer meets the
specifications of the Figure 2-2 or 2-3, the damage shall either be repaired to
restore proper alignment of the face openings, or the tube shall be discarded.
4.1.6.2.2 Pitot Tube Assemblies. After each field use, check the face opening
alignment of the pitot tube, as in Section 4.1.6.2.1; also, remeasure the
intercomponent spacings of the assembly. If the intercomponent spacings have not
changed and the face opening alignment is acceptable, it can be assumed that the
coefficient of the assembly has not changed. If the face opening alignment is
no longer within the specifications of Figure 2-2 or 2-3, either repair the
damage or replace the pitot tube (calibrating the new assembly, if necessary).
If the intercomponent spacings have changed, restore the original spacings, or
recalibrate the assembly.
4.2 Standard Pitot Tube (if applicable). If a standard pitot tube is used for
the velocity traverse, the tube shall be constructed according to the criteria
of Section 2.7 and shall be assigned a baseline coefficient value of 0.99. If
the standard pitot tube is used as part of an assembly, the tube shall be in an
interference-free arrangement (subject to the approval of the Administrator).
4.3 Temperature Gauges. After each field use, calibrate dial thermometers,
liquid-filled bulb thermometers, thermocouple-potentiometer systems, and other
gauges at a temperature within 10 percent of the average absolute stack
temperature. For temperatures up to 405°C (761°F) , use an ASTM mercury-in-glass
reference thermometer, or equivalent, as a reference; alternatively, either
a reference thermocouple and potentiometer (calibrated by NBS) or thermometric
fixed points, e.g., ice bath and boiling water (corrected for barometric
pressure) may be used. For temperatures above 405°C (761°F), use an NBS-
calibrated reference thermocouple-potentiometer system or an alternative
reference, subject to the approval of the Administrator.
If, during calibration, the absolute temperature measured with the gauge being
calibrated and the reference gauge agree within 1.5 percent, the temperature data
taken in the field shall be considered valid. Otherwise, the pollutant emission
test shall either be considered invalid or adjustments (if appropriate) of the
test results shall be made, subject to the approval of the Administrator.
4.4 Barometer. Calibrate the barometer used against a mercury barometer.
5. CALCULATIONS
Carry out calculations, retaining at least one extra decimal figure beyond that
of the acquired data. Round off figures after final calculation.
5.1 Nomenclature.
A = Cross-sectional area of stack, m2 (ft2) .
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EMTIC TM-002
NSPS TEST METHOD
Page 12
BWB = Water vapor in the gas stream (from Method 5 or Reference
Method 4), proportion by volume.
Cp = Pitot tube coefficient, dimensionless.
Kp = Pitot tube constant,
34.97
m
sec
(g/g-mole)(mmHg)
(mmH20)
1/2
for the metric system.
85.49
ft
sec
"ib/lb
(°
-mole)
R) (in
(in.
.H20)
Hg) "
1/2
for the English system.
M
-------
EMTIC TM-002
NSPS TEST METHOD
Page 13
for metric.
Absolute stack temperature, °K (°R)
= 273 + t.
= 460 + t.
Eq. 2-7
for English.
Ap
Eq. 2-8
Standard absolute temperature, 293°K (528°R).
Average stack gas velocity, m/sec (ft/sec).
Velocity head of stack gas, mm H20 (in. H20) .
3,600= Conversion factor, sec/hr.
18.0 = Molecular weight of water, g/g-mole (Ib/lb-mole).
5.2 Average Stack Gas Velocity.
\
s(avg)
Eq. 2-9
5.3 Average Stack Gas Dry Volumetric Flow Rate.
T
Qsd = 3,600(l-Bws)vsA
std
's(avg)
' std
BIBLIOGRAPHY
1. Mark, L.S. Mechanical Engineers' Handbook. New York.
Co., Inc. 1951.
Eq. 2-10
McGraw-Hill Book
2. Perry. J.H. Chemical Engineers' Handbook. New York. McGraw-Hill Book
-------
EMTIC TM-002 NSPS TEST METHOD Page 14
Co., Inc. 1960.
3. Shigehara, R.T., W.F. Todd, and W.S. Smith. Significance of Errors in
Stack Sampling Measurements. U.S. Environmental Protection Agency,
Research Triangle Park, N.C. (Presented at the Annual Meeting of the Air
Pollution Control Association, St. Louis, MO., June 14-19, 1970).
4. Standard Method for Sampling Stacks for Particulate Matter. In: 1971 Book
of ASTM Standards, Part 23. Philadelphia, PA. 1971. ASTM Designation
D 2928-71.
5. Vennard, J.K. Elementary Fluid Mechanics. New York. John Wiley and Sons,
Inc. 1947.
6. Fluid Meters - Their Theory and Application. American Society of
Mechanical Engineers, New York, N.Y. 1959.
7. ASHRAE Handbook of Fundamentals. 1972. p. 208.
8. Annual Book of ASTM Standards, Part 26. 1974. p. 648.
9. Vollaro, R.F. Guidelines for Type S Pitot Tube Calibration. U.S.
Environmental Protection Agency, Research Triangle Park, N.C. (Presented
at 1st Annual Meeting, Source Evaluation Society, Dayton, OH,
September 18, 1975.)
10. Vollaro, R.F. A Type S Pitot Tube Calibration Study. U.S. Environmental
Protection Agency, Emission Measurement Branch, Research Triangle Park,
N.C. July 1974.
11. Vollaro, R.F. The Effects of Impact Opening Misalignment on the Value of
the Type S Pitot Tube Coefficient. U.S. Environmental Protection Agency,
Emission Measurement Branch, Research Triangle Park, NC. October 1976.
12. Vollaro, R.F. Establishment of a Baseline Coefficient Value for Properly
Constructed Type S Pitot Tubes. U.S. Environmental Protection Agency,
Emission Measurement Branch, Research Triangle Park, NC. November 1976.
13. Vollaro, R.F. An Evaluation of Single-Velocity Calibration Technique as a
Means of Determining Type S Pitot Tube Coefficients. U.S. Environmental
Protection Agency, Emission Measurement Branch, Research Triangle Park, NC.
August 1975.
14. Vollaro, R.F. The Use of Type S Pitot Tubes for the Measurement of Low
Velocities. U.S. Environmental Protection Agency, Emission Measurement
Branch, Research Triangle Park, NC. November 1976.
15. Smith, Marvin L. Velocity Calibration of EPA Type Source Sampling Probe.
United Technologies Corporation, Pratt and Whitney Aircraft Division, East
Hartford, CT. 1975.
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EMTIC TM-002 MSPS TEST METHOD Page 15
16. Vollaro, R.F. Recommended Procedure for Sample Traverses in Ducts Smaller
than 12 Inches in Diameter. U.S. Environmental Protection Agency, Emission
Measurement Branch, Research Triangle Park, NC. November 1976.
17. Ower, E. and R.C. Pankhurst. The Measurement of Air Flow, 4th Ed. London,
Pergamon Press. 1966.
18. Vollaro, R.F. A Survey of Commercially Available Instrumentation for the
Measurement of Low-Range Gas Velocities. U.S. Environmental Protection
Agency, Emission Measurement Branch, Research Triangle Park, NC.
November 1976. (Unpublished Paper).
19. Gnyp, A.W., C.C. St. Pierre, D.S. Smith, D. Mozzon, and J. Steiner. An
Experimental Investigation of the Effect of Pitot Tube-Sampling Probe
Configurations on the Magnitude of the S Type Pitot Tube Coefficient for
Commercially Available Source Sampling Probes. Prepared by the University
of Windsor for the Ministry of the Environment, Toronto, Canada.
February 1975.
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EMTIC TM-002
NSPS TEST METHOD
Page 16
1.90 -2.64 cm*
(0.75-1.0 In.)
7.62 em (3 in.)'
Temperature Sensor
Type S PKot Tube
* Suggested (Inttrtaranc* Frae)
PKol tube/Thermocouple Spicing
Figure 2-1. Type S pi tot tube manometer assembly.
-------
EMTIC TM-002
NSPS TBST METHOD
Page 17
Transverse
Tub* Aid*
Longltudlnil
Tube Axit
A-Slde Plan*
PI A
B-SkJe Plant
fT AorB V J
(c)
(a) and vtaw; faca opening planet perpendicular
to trantvertt axlt;
(b) top view; face opening planet parallel to
longitudinal axlt:
(c) iMa view: both leg! of equal length and
bolhildu. BateHne coefficient rakm of
0.64 may be attigned to pMottubet con-
ttnictod Vila way
Figure 2-2. Properly constructed Type S pi tot tube.
-------
EMTIC TM-002
NSPS TBST METHOD
Page 18
•4-
_ _ -JT-=a-O_ —
-
rri-3
Figure 2-3. Types of face-opening misalignment that can result from field use
or improper construction of Type S pitot tubes. These will not affect the
baseline value of Cp(s) so long as a1 and a2 £10°, P1 and (52 s5°, z so.32 cm (1/8
in.) and w sO.08 cm (1/32 in.) (citation 11 in Bibliography).
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EMTIC TM-002
NSPS TEST METHOD
Page 19
Curvtdor
lUwwt Junction
Stittc
Hotai
(-0.1D) '
H.mfcplwrtol _
Tip
Figure 2-4. Standard pi tot tube design specifications.
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EMTIC TM-002 NSPS TEST METHOD Page 20
-------
EMTIC TM-002
NSPS TKST METHOD
Page 21
PLANT
DATE
DIMENSIONS,
(in. Hg) _
OPERATORS _
PITOT TUBE
RUN NO.
(in.) _
.STACK DIA. OR
m (in.) BAROMETRIC PRESS., mm Hg
_CROSS SECTIONAL AREA, m2 (ft2)
I.D. NO.
AVG. COEFFICIENT,
Cp
LAST DATE CALIBRATED
SCHEMATIC OF STACK
CROSS SECTION
Traverse
Pt. No.
Vel. Hd. , Ap
mm ( in . ) H2O
Stack Temperature
TB,
°C (°F)
Average
T»,
°K (°R)
P3
mm Hg
(in.Hg)
(AP) i/a
Figure 2-5. Velocity traverse data.
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EMTIC TM-002
NSPS TEST METHOD
Page 22
Tn»8PiotTyb«
A >E1M«B(Mh.)toD 10 —
Samplng Nozzte
A. Bottom View; ihowlng minimum pKot tub*-nozzl* np«r»tlon.
Typ.S
PltotTubi
B. Side Vtow; to pravint pilot tub* from Intwlortng with gu
flow •tmimliruM ipproichlng th* nozzto, th* tmpict pratiura
opening plini of the pKot tub* ihitt be even with or *bov* the
nozzto *ntry plan*.
Figure 2-6. Proper pi tot tube-sampling nozzle configuration to prevent
aerodynamic interference; button-hook type nozzle; centers of nozzle and
pitot opening aligned; Dt between 0.48 and 0.95 cm (3/16 and 3/8 in.).
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EMTIC TM-002
NSPS TEST METHOD
Page 23
|o, TH>. s p«ot TUI
Swnpfe Prate
I OR
I
I
Figure 2-7. Proper thermocouple placement to prevent interference; Dt
between 0.48 and 0.95 cm (3/16 and 3/8 in.).
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EMTIC TM-002
NSPS TEST METHOD
Page 24
D, Type S Pilot Tube
Sample Probe
Figure 2-8. Minimum pitot-sample probe separation needed to prevent
interference; Dt between 0.48 and 0.95 cm (3/16 and 3/8 in.).
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EMTIC TM-002
NSPS TEST METHOD
Page 25
PITOT TUBE IDEN1
RUN NO.
1
2
3
IFICATION NUMBEI
"A
cm H2O
(in H2O)
I : DATE
1 SIDE CALIBRATI
cm H2O
(in H20)
Cp.avg
(SIDE A)
: CJ
ON
VIBRATED BY:
Deviation
Cp,., - Cp(A)
RUN NO.
1
2
3
"B" SIDE CALIBRATION
APstd
cm H20
(in H2O)
AP
cm H20
(in H2O)
r
^p, avg
(SIDE B)
Cp(S>
Deviation
Cp,., - Cp(B)
Average Deviation = a
'p(s) p(AorB)
(AorB)
•MustBe^O.Ol
C (SideA)-C (SideB)
•MustBe^O.Ol
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EMTIC TM-002 NSPS TKST HKTHOD Page 26
Figure 2-9. Pitot tube calibration data.
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EMTIC TM-002
NSPS TEST METHOD
Page 27
Figure 2-10. Projected-area models for typical pitot tube assemblies,
-------
Appendix G.3
EPA Method 3A
-------
EMISSION MEASUREMENT TECHNICAL INFORMATION CENTER
NSPS TEST METHOD
Method 3A • Determination of Oxygen and Carbon Dioxide Concentrations
1n Emissions fron Stationary Sources
(Instnnental Analyzer Procedure)
1. APPLICABILITY AND PRINCIPLE
1.1 Applicability. This method 1s applicable to the determination of oxygen (02) and
carbon dioxide (COj) concentrations 1n emissions from stationary sources only when
specified within the regulations.
1.2 Principle. A sample 1s continuously extracted from the effluent stream: a
portion of the sample stream 1s conveyed to an Instrumental analyzer(s) for
determination of 02 and CQ concentration(s). Performance specifications and test
procedures are provided to ensure reliable data.
2. RANGE AND SENSITIVITY
Same as in Method 6C. Sections 2.1 and 2.2. except that the span of the monitoring
system shall be selected such that the average 02 or C02 concentration is not less than
20 percent of the span.
3. DEFINITIONS
3.1 Measurement System. The total equipment required for the determination of the 02
or COj concentration. The measurement system consists of the same major subsystems as
defined in Method 6C. Sections 3.1.1. 3.1.2. and 3.1.3.
3.2 Span. Calibration Gas. Analyzer Calibration Error, Sampling System Bias. Zero
Drift. Calibration Drift. Response Time, and Calibration Curve. Same as in Method 6C.
Sections 3.2 through 3.8. and 3.10.
3.3 Interference Response. The output response of the measurement system to a
component in the sample gas. other than the gas component being measured.
4. MEASUREMENT SYSTEM PERFORMANCE SPECIFICATIONS
Same as in Method 6C. Sections 4.1 through 4.4.
Prepared by Emission Measurement Branch EMTIC TM-003A
Technical Support Division. OAQPS. EPA May 6. 1989
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EMTIC TM-003A NSPS TEST METHOD Page 2
5. APPARATUS AND REAGENTS
*
5.1 Measurement Systen. Any measurement system for 02 or CQ that meets the
specifications of this method. A schematic of an acceptable measurement system 1s
shown in Figure 6C-1 of Method 6C. The essential components of the measurement system
are described below:
5.1.1 Sample Probe. A leak-free probe of sufficient length to traverse the sample
points.
5.1.2 Sample Line. Tubing to transport the sample gas from the probe to the moisture
removal system. A heated sample line 1s not required for systems that measure the 02
or C02 concentration on a dry basis, or transport dry gases.
5.1.3 Sample Transport Line. Calibration Valve Assembly. Moisture Removal System.
Participate Filter. Sample Pump. Sample Flow Rate Control. Sample Gas Manifold, and
Data Recorder. Same as in Method 6C. Sections 5.1.3 through 5.1.9. and 5.1.11. except
that the requirements to use stainless steel. Teflon, and nonreactlve glass filters do
not apply.
5.1.4 Gas Analyzer. An analyzer to determine continuously the Qj, or CO* concentration
in the sample gas stream. The analyzer must meet the applicable performance
specifications of Section 4. A means of controlling the analyzer flow rate and a
device for determining proper sample flow rate (e.g.. precision rotameter. pressure
gauge downstream of all flow controls, etc.) shall be provided at the analyzer. The
requirements for measuring and controlling the analyzer for measuring and controlling
the analyzer flow rate are not applicable if data are presented that demonstrate the
analyzer is insensitive to flow variations over the range encountered during the test.
5.2 Calibration Gases. The calibration gases for COj analyzers shall be C02 1n NZ or
COz in air. Alternatively. COz/SOz. 02/SOz, or (yoysOz gas mixtures in N2 may be used.
Three calibration gases, as specified in Sections 5.3.1 through 5.3.4 of Method 6C.
shall be used. For 02 monitors that cannot analyze zero gas. a calibration gas
concentration equivalent to less than 10 percent of the span may be used in place of
zero gas.
6. MEASUREMENT SYSTEM PERFORMANCE TEST PROCEDURES
Perform the following procedures before measurement of emissions (Section 7).
6.1 Calibration Concentration Verification. Follow Section 6.1 of Method 6C. except
1f calibration gas analysis is required, use Method 3 and change the acceptance
criteria for agreement among Method 3 results to 5 percent (or 0.2 percent by volume.
whichever is greater).
6.2 Interference Response. Conduct an Interference response test of the analyzer
prior to Its Initial use 1n the field. Thereafter, recheck the measurement system if
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EMTIC TM-003A NSPS TEST METHOD Page 3
changes are made 1n the instrumentation that could alter the Interference response
(e.g., changes in the type of gas detector). Conduct the interference response in
accordance with Section 5.4 of Method 20.
6.3 Measurement System Preparation. Analyzer Calibration Error, Response Time, and
Sampling System Bias Check. Follow Sections 6.2 through 6.4 of Method 6C.
7. EMISSION TEST PROCEDURE
7.1 Selection of Sampling Site and Sampling Points. Select a measurement site and
sampling points using the same criteria that are applicable to tests performed using
Method 3.
7.2 Sample Collection. Position the sampling probe at the first measurement point.
and begin sampling at the same rate as that used during the response time test.
Maintain constant rate sampling (i.e.. ±10 percent) during the entire run. The
sampling time per run shall be the same as for tests conducted using Method 3 plus
twice the average system response time. For each run. use only those measurements
obtained after twice the response time of the measurement system has elapsed to
determine the average effluent concentration.
7.3 Zero and Calibration Drift Test. Follow Section 7.4 of Method 6C.
8. QUALITY CONTROL PROCEDURES
The following quality control procedures are recoirmended when the results of this
method are used for an emission rate correction factor, or excess air determination.
The tester should select one of the following options for validating measurement
results:
8.1 If both 02 and CQ are measured using Method 3A. the procedures described in
Section 4.4 of Method 3 should be followed to validate the Oz and CQ measurement
results.
8.2 If only 02 is measured using Method 3A. measurements of the sample stream 2CO
concentration should be obtained at the sample by-pass vent discharge using an Orsat
or Fyrite analyzer, or equivalent. Duplicate samples should be obtained concurrent
with at least one run. Average the duplicate Orsat or Fyrite analysis results for
each run. Use the average C02 values for comparison with thez 0 measurements in
accordance with the procedures described in Section 4.4 of Method 3.
8.3 If only C02 is measured using Method 3A. concurrent measurements of the sample
stream C02 concentration should be obtained using an Orsat or Fyrite analyzer as
described in Section 8.2. For each run. differences greater than 0.5 percent between
the Method 3A results and the average of the duplicate Fyrite analysis should be
investigated.
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EMTIC TM-003A NSPS TEST METHOD Page 4
9. EMISSION CALCULATION
9.1 For all C02 analyzers, and for Oj analyzers that can be calibrated with zero gas.
follow Section 8 of Method 6C. except express all concentrations as percent, rather
than ppm.
9.2 For Oz analyzers that use a low-level calibration gas 1n place of a zero gas.
calculate the effluent gas concentration using Equation 3A-1.
C.-GO,
(C - C.) -K^ Eq. 3A-1
c.-c0
Where:
' Gg»$ " Effluent gas concentration, dry basis, percent.
C., - Actual concentration of the upscale calibration gas. percent.
CM - Actual concentration of the low-level calibration gas. percent.
C. - Average of initial and final system calibration bias check
responses for the upscale calibration gas. percent.
C0 - Average of initial and final system calibration bias check
responses for the low level gas. percent.
U - Average gas concentration indicated by the gas analyzer, dry basis.
percent.
10. BIBLIOGRAPHY
Same as in Bibliography of Method 6C.
-------
Appendix G.4
EPA Method 4
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EMISSION MEASUREMENT TECHNICAL INFORMATION CENTER
NSPS TEST METHOD
Method 4 - Determination of Moisture Content
in Stack Gases
1. PRINCIPLE AND APPLICABILITY
1.1 Principle. A gas sample is extracted at a constant rate from
the source; moisture is removed from the sample stream and
determined either volumetrically or gravimetrically.
*
1.2 Applicability. This method is applicable for determining the
moisture content of stack gas.
1.2.1 Two procedures are given. The first is a reference method,
for accurate determinations of moisture content (such as are needed
to calculate emission data). The second is an approximation
method, which provides estimates of percent moisture to aid in
setting isokinetic sampling rates prior to a pollutant emission
measurement run. The approximation method described herein is only
a suggested approach; alternative means for approximating the
moisture content, e.g., drying tubes, wet bulb-dry bulb techniques,
condensation techniques, stoichiometric calculations, previous
experience, etc., are also acceptable.
1.2.2 The reference method is often conducted simultaneously with
a pollutant emission measurement run; when it is, calculation of
percent isokinetic, pollutant emission rate, etc., for the run
shall be based upon the results of the reference method or its
equivalent; these calculations shall not be based upon the results
of the approximation method, unless the approximation method is
Prepared by Emission Measurement Branch EMTIC TM-004
Technical Support Division, OAQPS, EPA July 11, 1989
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EMISSION MEASUREMENT TECHNICAL INFORMATION CENTER
NSPS TEST METHOD
shown, to the satisfaction of the Administrator, U.S. Environmental
Protection Agency, to be capable of yielding results within 1
percent H20 of the reference method.
1.2.3 Note: The reference method may yield questionable results
when applied to saturated gas streams or to streams that contain
water droplets. Therefore, when these conditions exist or are
suspected, a second determination of the moisture content shall be
made simultaneously with the reference method, as follows: Assume
that the gas stream is saturated. Attach a temperature sensor
[capable of measuring to within 1°C (2°F)] to the reference method
probe. Measure the stack gas temperature at each traverse point
(see Section 2.2.1) during the reference method traverse; calculate
the average stack gas temperature. Next, determine the moisture
percentage, either by: (1) using a psychrometric chart and making
appropriate corrections if stack pressure is different from that of
the chart, or (2) using saturation vapor pressure tables. In cases
where the psychrometric chart or the saturation vapor pressure
tables are not applicable (based on evaluation of the process),
alternative methods, subject to the approval of the Administrator,
shall be used.
2. REFERENCE METHOD
The procedure described in Method 5 for determining moisture
content is acceptable as a reference method.
2.1 Apparatus. A schematic of the sampling train used in this
reference method is shown in Figure 4-1. All components shall be
maintained and calibrated according to the procedures in Method 5.
Prepared by Emission Measurement Branch EMTIC TM-004
Technical Support Division, OAQPS, EPA July 11, 1989
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EMTIC TM-004 EMTIC NSPS TEST METHOD
Page 3
2.1.1 Probe. Stainless steel or glass tubing, sufficiently heated
to prevent water condensation, and equipped with a filter, either
in-stack (e.g., a plug of glass wool inserted into the end of the
probe) or heated out-stack (e.g., as described in Method 5), to
remove particulate matter. When stack conditions permit, other
metals or plastic tubing may be used for the probe, subject to the
approval of the Administrator.
2.1.2 Condenser. See Method 5, Section 2.1.7, for a description
of an acceptable type of condenser and for alternative measurement
systems.
2.1.3 Cooling System. An ice bath container and crushed ice (or
equivalent), to aid in condensing moisture.
2.1.4 Metering System. Same as in Method 5, Section 2.1.8, except
do not use sampling systems designed for flow rates higher than
0.0283 m3/min (1.0 cfm). Other metering systems, capable of
maintaining a constant sampling rate to within 10 percent and
determining sample gas volume to within 2 percent, may be used,
subject to the approval of the Administrator.
2.1.5 Barometer. Mercury, aneroid, or other barometer capable of
measuring atmospheric pressure to within 2.5 mm (0.1 in.) Hg. See
NOTE in Method 5, Section 2.1.9.
2.1.6 Graduated Cylinder and/or Balance. To measure condensed
water and moisture caught in the silica gel to within 1 ml or 0.5
g. Graduated cylinders shall have subdivisions no greater than 2
ml. Most laboratory balances are capable of weighing to the
nearest 0.5 g or less. These balances are suitable for use here.
2.2 Procedure. The following procedure is written for a condenser
system (such as the impinger system described in Section 2.1.7 of
Method 5) incorporating volumetric analysis to measure the
condensed moisture, and silica gel and gravimetric analysis to
measure the moisture leaving the condenser.
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EMTIC TM-004 EMTIC NSPS TEST METHOD
Page 4
2.2.1 Unless otherwise specified by the Administrator, a minimum
of eight traverse points shall be used for circular stacks having
diameters less than 0.61 m (24 in.), a minimum of nine points shall
be used for rectangular stacks
having equivalent diameters less than 0.61 m (24 in.), and a
minimum of twelve traverse points shall be used in all other cases.
The traverse points shall be located according to Method 1. The
use of fewer points is subject to the approval of the
Administrator. Select a suitable probe and probe length such that
all traverse points can be sampled. Consider sampling from
opposite sides
of 'the stack (four total sampling ports) for large stacks, to
permit use of shorter probe lengths. Mark the probe with heat
resistant tape or by some other method to denote the proper
distance into the stack or duct for each sampling point. Place
known volumes of water in the first two impingers. Weigh and
record the weight of the silica gel to the nearest 0.5 g, and
transfer the silica gel to the fourth impinger; alternatively, the
silica gel may first be transferred to the impinger, and the weight
of the silica gel plus impinger recorded.
2.2.2 Select a total sampling time such that a minimum total gas
volume of 0.60 scm (21 scf) will be collected, at a rate no greater
than 0.021 m3/min (0.75 cfm) . When both moisture content and
pollutant emission rate are to be determined, the moisture
determination shall be simultaneous with, and for the same total
length of time as, the pollutant emission rate run, unless
otherwise specified in an applicable subpart of the standards.
2.2.3 Set up the sampling train as shown in Figure 4-1. Turn on
the probe heater and (if applicable) the filter heating system to
temperatures of about 120°C (248°F), to prevent water condensation
ahead of the condenser; allow time for the temperatures to
stabilize. Place crushed ice in the ice bath container. It is
recommended, but not required, that a leak check be done, as
follows: Disconnect the probe from the first impinger or (if
applicable) from the filter holder. Plug the inlet to the first
impinger (or filter holder), and pull a 380 mm (15 in.) Hg vacuum;
a lower vacuum may be used, provided that it is not exceeded during
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EMTIC TM-004 EMTIC NSPS TEST METHOD
Page 5
the test. A leakage rate in excess of 4 percent of the average
sampling rate or 0.00057 m3/min (0.02 cfm), whichever is less, is
unacceptable. Following the leak check, reconnect the probe to the
sampling train.
2.2.4 During the sampling run, maintain a sampling rate within 10
percent of constant rate, or as specified by the Administrator.
For each run, record the data required on the example data sheet
shown in Figure 4-2. Be sure to record the dry gas meter reading
at the beginning and end of each sampling time increment and
whenever sampling is halted. Take other appropriate readings at
each sample point, at least once during each time increment.
2.2.5 To begin sampling, position the probe tip at the first
traverse point. Immediately start the pump, and adjust the flow to
the desired rate. Traverse the cross section, sampling at each
traverse point for an equal length of time. Add more ice and, if
necessary, salt to maintain a temperature of less than 20°C (68°F)
at the silica gel outlet.
2.2.6 After collecting the sample, disconnect the probe from the
filter holder (or from the first impinger), and conduct a leak
check (mandatory) as described in Section 2.2.3. Record the leak
rate. If the leakage rate exceeds the allowable rate, the tester
shall either reject the test results or shall correct the sample
volume as in Section 6.3 of Method 5. Next, measure the volume of
the moisture condensed to the nearest ml. Determine the increase
in weight of the silica gel (or silica gel plus impinger) to the
nearest 0.5 g. Record this information (see example data sheet,
Figure 4-3) , and calculate the moisture percentage, as described in
2.3 below.
2.2.7 A quality control check of the volume metering system at the
field site is suggested before collecting the sample following the
procedure in Method 5, Section 4.4.
2.3 Calculations. Carry out the following calculations, retaining
at least one extra decimal figure beyond that of the acquired data.
Round off figures after final calculation.
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EMTIC TM-004 EMTIC NSPS TEST METHOD
Page 6
2.3.1 Nomenclature.
Bws = Proportion of water vapor, by volume, in the gas stream.
Mw = Molecular weight of water, 18.0 g/g-mole (18.0 Ib/lb-
mole).
Pm = Absolute pressure (for this method, same as barometric
pressure) at the dry gas meter, mm Hg (in. Hg) .
Pstd = Standard absolute pressure, 760 mm Hg (29.92 in. Hg) .
R = Ideal gas constant, 0.06236 (mm Hg) (m3) / (g-mole) (°K) for
metric units and 21.85 (in. Hg) (ft3) / (Ib-mole) (°R) for
English units.
Tm = Absolute temperature at meter, °K (°R) .
Tgtd = Standard absolute temperature, 293°K (528°R) .
Vra = Dry gas volume measured by dry gas meter, dcm (dcf).
AVm = Incremental dry gas volume measured by dry gas meter at
each traverse point, dcm (dcf).
Vm(std) = DrY 9as volume measured by the dry gas meter, corrected to
standard conditions, dscm (dscf).
vwc(std> = Volume of water vapor condensed, corrected to standard
conditions, scm (scf).
VWSg(std) = Volume of water vapor collected in silica gel, corrected
to standard conditions, scm (scf).
Vf = Final volume of condenser water, ml.
Vi = Initial volume, if any, of condenser water, ml.
Wf = Final weight of silica gel or silica gel plus impinger, g.
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EMTIC TM-004 EMTIC NSPS TEST METHOD
Page 7
Wi = Initial weight of silica gel or silica gel plus impinger,
g-
Y = Dry gas meter calibration factor.
pw = Density of water, 0.9982 g/ml (0.002201 Ib/ml).
2.3.2 Volume of Water Vapor Condensed.
RT
V , _ = (V -V )p std
wc(std) fi'wFM Eq.4-1
std w ^
Where :
K! = 0.001333 m3/ml for metric units,
= 0.04707 ftYml for English units.
2.3.3 Volume of Water Collected in Silica Gel
_ (Wf - W,) RTgtd
wsg(std) PstdMw E(3- 4~2
= K2 (Wf - WJ
Where :
K2 = 0.001335 m3/g for metric units,
= 0.04715 ft3/g for English units
2.3.4 Sample Gas Volume .
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EMTIC TM-004 EMTIC NSPS TEST METHOD
Page 8
(P )(T )
V = V Y —
m(std) m /p v / m \
VStP " E^- 4-3
= K Y _!LJi
3 T,
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EMTIC TM-004 EMTIC NSPS TEST METHOD
Page 9
Where:
K3 = 0.3858 °K/mm Hg for metric units,
= 17.64 °R/in. Hg for English units
NOTE: If the post-test leak rate (Section 2.2.6) exceeds the
allowable rate, correct the value of Vra in Equation 4-3, as
described in Section 6.3 of Method 5.
2.3*.5 Moisture Content.
-. wc(std) wsg(std) Eq. 4-4
ws v +v +v
wc(std) wsg(std) jn(std)
NOTE: In saturated or moisture droplet-laden gas streams, two
calculations of the moisture content of the stack gas shall be
made, one using a value based upon the saturated conditions (see
Section 1.2), and another based upon the results of the impinger
analysis. The lower of these two values of Bws shall be considered
correct.
2.3.6 Verification of Constant Sampling Rate. For each time
increment, determine the AVm. Calculate the average. If the value
for any time increment differs from the average by more than 10
percent, reject the results, and repeat the run.
3. APPROXIMATION METHOD
The approximation method described below is presented only as a
suggested method (see Section 1.2).
3.1 Apparatus. See Figure 4-4.
3.1.1 Probe. Stainless steel or glass tubing, sufficiently heated
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EMTIC TM-004 EMTIC NSPS TEST METHOD
Page 10
to prevent water condensation and equipped with a filter (either
in-stack or heated out-stack) to remove particulate matter. A plug
of glass wool, inserted into the end of the probe, is a
satisfactory filter.
3.1.2 Impingers. Two midget impingers, each with 30-ml capacity,
or equivalent.
3.1.3 Ice Bath. Container and ice, to aid in condensing moisture
in impingers.
3.1.'4 Drying Tribe. Tube packed with new or regenerated 6- to 16-
mesh indicating-type silica gel (or equivalent desiccant), to dry
the sample gas and to protect the meter and pump. .
3.1.5 Valve. Needle valve, to regulate the sample gas flow rate.
3.1.6 Pump. Leak-free, diaphragm type, or equivalent, to pull the
gas sample through the train.
3.1.7 Volume Meter. Dry gas meter, sufficiently accurate to
measure the sample volume to within 2 percent, and calibrated over
the range of flow rates and conditions actually encountered during
sampling.
3.1.8 Rate Meter. Rotameter, to measure the flow range from 0 to
3 liters/min (0 to 0.11 cfm).
3.1.9 Graduated Cylinder. 25-ml.
3.1.10 Barometer. Mercury, aneroid, or other barometer, as
described in Section 2.1.5 above.
3.1.11 Vacuum Gauge. At least 760-mm (30-in.) Hg gauge, to be
used for the sampling leak check.
3.2 Procedure.
3.2.1 Place exactly 5 ml water in each impinger. Leak check the
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EMTIC TM-004 EMTIC NSPS TEST METHOD
Page 11
sampling train as follows: Temporarily insert a vacuum gauge at or
near the probe inlet; then, plug the probe inlet, and pull a vacuum
of at least 250 mm (10 in.) Hg. Note the time rate of change of
the dry gas meter dial; alternatively, a rotameter (0 to 40 cc/min)
may be temporarily attached to the dry gas meter outlet to
determine the leakage rate. A leak rate not in excess of 2 percent
of the average sampling rate is acceptable. NOTE: Carefully
release the probe inlet plug before turning off the pump.
3.2.2 Connect the probe, insert it into the stack, and sample at
a constant rate of 2 liters/min (0.071 cfm). Continue sampling
until the dry gas meter registers about 30 liters (1.1 ft3) or
until visible liquid droplets are carried over from the first
impinger to the second. Record temperature, pressure, and dry gas
meter readings as required by Figure 4-5.
3.2.3 After collecting the sample, combine the contents of the two
impingers, and measure the volume to the nearest 0.5 ml.
3.3 Calculations. The calculation method presented is designed to
estimate the moisture in the stack gas; therefore, other data,
which are only necessary for accurate moisture determinations, are
not collected. The following equations adequately estimate the
moisture content, for the purpose of determining isokinetic
sampling rate settings.
3.3.1 Nomenclature.
Bwm = Approximate proportion by volume of water vapor in the gas
stream leaving the second impinger, 0.025.
Bws = Water vapor in the gas stream, proportion by volume.
Mw = Molecular weight of water, 18.0 g/g-mole (18.0 Ib/lb-
mole).
Pm = Absolute pressure (for this method, same as barometric
pressure) at the dry gas meter, mm Hg (in. Hg).
-------
EMTIC TM-004 EMTIC NSPS TEST METHOD
Page 12
Pstd = Standard absolute pressure, 760 mm Hg (29.92 in. Hg) .
R = Ideal gas constant, 0.06236 [(mm Hg) (m3) ] / [ (g-mole) (°K) 3
for metric units and 21.85 [(in. Hg) (ft3) ] / [ (Ib-mole) (°R)]
for English units.
Tra = Absolute temperature at meter, °K (°R) .
Tstd = Standard absolute temperature, 293°R (528°R) .
Vf = Final volume of impinger contents, ml.
Vi = Initial volume of impinger contents, ml.
Vm = Dry gas volume measured by dry gas meter, dcm (dcf ) .
Vm(Std) = Dry gas volume measured by dry gas meter, corrected to
standard conditions, dscm (dscf) .
Y = Dry gas meter calibration factor.
pw = Density of water, 0.9982 g/ml (0.002201 Ib/ml) .
3.3.2 Volume of Water Vapor Collected.
PstdMw Eg. 4-5
= 1^(7, -V±)
Where :
K! = 0.001333 m3/ml for metric units,
= 0.04707 ft3/ml for English units
3.3.3 Gas Volume.
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EMTIC TM-004 EMTIC NSPS TEST METHOD
Page 13
T
X
m(std) m| I I T
»td/ V » / Ea. 4-6
Pm
= K, Vm -S
2 mm
Where:
K2 = 0.03858 °K/mm Hg for metric units,
= 17.64 °R/in. Hg for English units.
3.3.4 Approximate Moisture Content.
B = +B
ws V +V vm
we m(std) g—. 4-7
= — + (0.025)
V +V
we m(std)
4. CALIBRATION
4.1 For the reference method, calibrate the metering system,
temperature gauges, and barometer according to Sections 5.3, 5.5,
and 5.7, respectively, of Method 5. The recommended leak check of
the metering system (Section 5.6 of Method 5) also applies to the
reference method. For the approximation method, use the procedures
outlined in Section 5.1.1 of Method 6 to calibrate the metering
system, and the procedure of Method 5, Section 5.7, to calibrate
the barometer.
5. BIBLIOGRAPHY
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EMTIC TM-004 EMTIC NSPS TEST METHOD
Page 14
1. Air Pollution Engineering Manual (Second Edition). Danielson,
J.A. (ed.). U.S. Environmental Protection Agency, Office of Air
Quality Planning and Standards. Research Triangle Park, NC.
Publication No. AP-40. 1973.
2. Devorkin, Howard, et al. Air Pollution Source Testing Manual.
Air Pollution Control District, Los Angeles, CA. November 1963.
3. Methods for Determination of Velocity, Volume, Dust and Mist
Content of Gases. Western Precipitation Division of Joy
Manufacturing Co. Los Angeles, CA. Bulletin WP-50. 1968.
-------
EMTIC TM-004
EMTIC NSPS TEST METHOD
Page 15
Filter
(Either In Stick)
or Out of Stack)
CondenaeMee Bath System Including SWea OelTube
method.
Figure 4-1. Moisture sampling train reference
-------
EMTIC TM-004 EMTIC NSPS TEST METHOD
Page 16
-------
Figure 4-2. Field Moisture Determination Reference Method.
Plant
Location,
Operator.
Date
Run No.
Ambient temperature.
Barometric pressure.
Probe Length
SCHEMATIC OF STACK CROSS SECTION
Traverse
Pt. No.
Sampling
Time
(6) , min
Stack
Temperature
°C (°F)
Average
Pressure
differential across
orifice meter AH
mm { in . ) H20
Meter
Reading gas
sample
volume
m3 (ft3)
AVn
m3
(ft3)
Gas sample
temperature at
dry gas meter
Inlet
Tmtn
°C(°F)
Outlet
TnW
°C(°F)
Temperature
of gas
leaving
condenser or
last
impinger
°C(°F)
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EMTIC TM-004 EMTIC NSPS TEST METHOD
Page 18
Figure 4-3. Analytical data - reference method.
Impinger Silica gel
volume. ml weight. a
Final
Initial
Difference
-------
EMTIC TM-004
EMTIC NSPS TEST METHOD
Page 19
\
UUg>t
Pun*
Figure 4-4. Moisture Samping Train - Approximation Method.
-------
EMTIC TM-004
EMTIC NSPS TEST METHOD
Page 20
Figure 4-5. Field Moisture Determination - Approximation Method.
Location.
Test
Date
Operator
Barometric pressure.
Comments:
Clock Time
«
Gas volume
through
meter, (V.) ,
m3 (ft3)
Rate meter
setting m3/min
(ftVmin)
Meter
temperature
0 C (° F)
-------
Appendix G.5
EPA Method 23
-------
6560-50
ENVIRONMENTAL PROTECTION AGENCY
40 CFR Part 60
[AD-FRL- ]
STANDARDS OF PERFORMANCE FOR NEW STATIONARY SOURCES
Appendix A , Test Method 23
AGENCY: Environmental Protection Agency (EPA) .
ACTION: Proposed Rule.
SUMMARY: This rule amends Method 23, entitled
"Determination of Polychlorinated Dibenzo-p-Dioxins and
Polychlorinated Dibenzofurans from Stationary Sources," to
*
correct existing errors in the method, to eliminate the methylene
chloride rinse of the sampling train, and to clarify the quality
assurance requirements of the method.
DATES: Comments. Comments must be received on or before
(90 days after publication in the FEDERAL
REGISTER].
Public Hearing. If anyone contacts EPA requesting to speak
at a public hearing by (two weeks after
publication in the FEDERAL REGISTER), a public hearing will be
held on (four weeks after publication in the
FEDERAL REGISTER), beginning at 10:00 a.m. Persons interested in
attending the hearing should call Ms. Lala Cheek at
(919) 541-5545 to verify that a hearing will be held.
Request to Speak at Hearing. Persons wishing to present
-------
oral testimony must contact EPA by (two weeks
after publication in the FEDERAL REGISTER).
ADDRESSES: Comments. Comments should be submitted (in duplicate
if possible) to Public Docket No. A-94-2 at the following
address: U. S. Environmental Protection Agency , Air and
Radiation Docket and Information Center, Mail Code: 6102, 401 M
Street, SW, Washington, DC 20460. The Agency requests that a
separate copy also be sent to the contact person listed below.
The docket is located at the above address in Room M-1500
•
Waterside Mall (ground floor), and may be inspected from
8:30 a.m. to Noon and 1:00 to 3:00 PM, Monday through Friday.
The proposed regulatory text and other materials related to this
rulemaking are available for review in the docket or copies may
be mailed on request from the Air Docket by calling 202-260-7548.
A reasonable fee may be charged for copying docket materials.
Public Hearing. If anyone contacts EPA requesting a public
hearing, it will be held at EPA's Emission Measurement
Laboratory, Research Triangle Park, North Carolina. Persons
interested in attending the hearing or wishing to present oral
testimony should notify Ms. Lala Cheek (MD-19), U.S.
Environmental Protection Agency, Research Triangle Park, North
Carolina 27711, telephone number (919) 541-5545.
-------
Docket: A Docket, A-94-22, containing materials relevant to
this rulemaking, is available for public inspection and copying
between 8:30 a.m. and Noon and 1:00 and 3:00 p.m., Monday through
Friday, in at EPA's Air Docket Section (LE-131), Room M-1500
Waterside Mall (ground floor) 401 M Street, S.W., Washington,
D.C. 20460. A reasonable fee may be charged for copying.
FOR FURTHER INFORMATION CONTACT: Gary McAlister, Emission
Measurement Branch (MD-19), Emissions, Monitoring, and Analysis
Division, U.S. Environmental Protection Agency, Research Triangle
Park, North Carolina 27711, telephone (919) 541-1062.
SUP PLEMENTARY INFORMATION:
The proposed regulatory text of the proposed rule is not
included in this Federal Register notice, but is available in
Docket No. A-94-22 or by written or telephone request from the
Air Docket (see ADDRESSES). If necessary, a limited number of
copies of the Regulatory Text are available from the EPA contact
persons designated earlier in this notice. This Notice with the
proposed regulatory language is also available on the Technology
Transfer Network (TTN), one of EPA's electronic bulletin boards.
TTN provides information and technology exchange in various areas
of air pollution control. The service is free except for the
cost of the phone call. Dial (919) 541-5742 for up to a 14400
-------
bps modem. If more information on TTN is needed, call the HELP
line at (919) 541-5384.
I. SUMMARY
Method 23 was promulgated along with the New Source
Performance Standard for municipal waste combustors (Subpart Ea).
As promulgated, the method contained some errors. This action
would correct those errors and would clarify some of the existing
quality assurance requirements. In addition, the current
procedure requires rinsing of the sampling train with two
*
separate solvents which must be analyzed separately. Based on
data the Agency has collected since promulgation of Method 23, we
believe that one of these rinse steps and the resulting sample
fraction can be eliminated. This could save as much as $2000 per
test run in analytical costs.
II. THE RULEMAKING
This rulemaking does not impose emission measurement
requirements beyond those specified in the current regulations
nor does it change any emission standard. Rather, the rulemaking
would simply amend an existing test method associated with
emission measurement requirements in the current regulations that
would apply irrespective of this rulemaking.
III. ADMINISTRATIVE REQUIREMENTS
-------
A. Public Hearing
A public hearing will be held, if requested, to discuss the
proposed amendment in accordance with section 307(d)(5)of the
Clean Air Act. Persons wishing to make oral presentations should
contact EPA at the address given in the ADDRESSES section of this
preamble. Oral presentations will be limited to 15 minutes each.
Any member of the public may file a written statement with EPA
before, during, or within 30 days after the hearing. Written
statements should be addressed to the Air Docket Section address
•
given in the ADDRESSES section of this preamble.
A verbatim transcript of the hearing and written statements
will be available for public inspection and copying during normal
working hours at EPA's Air Docket Section in Washington, DC (see
ADDRESSES section of this preamble).
B. Docket
The docket is an organized and complete file of all the
information considered by EPA in the development of this
rulemaking. The docket is a dynamic file, since material is
added throughout the rulemaking development. The docketing
system is intended to allow members of the public and industries
involved to identify and locate documents readily so that they
may effectively participate in the rulemaking process. Along
-------
with the statement of basis and purpose of the proposed and
promulgated test method revisions and EPA responses to
significant comments, the contents of the docket, except for
interagency review materials, will serve as the record in case of
judicial review [Section 307(d)(7)(A)].
C. Executive Order 12291 Review
Under Executive Order 12291, EPA is required to judge
whether a regulation is a "major rule" and, therefore, subject to
the requirements of a regulatory impact analysis. This
•
rulemaking does not impose emission measurement requirements
beyond those specified in the current regulations, nor does it
change any emission standard. The Agency has determined that
this regulation would result in none of the adverse economic
effects set forth in Section 1 of the Order as grounds for
finding the regulation to be a "major rule." The Agency has,
therefore, concluded that this regulation is not a "major rule"
under Executive Order 12291.
D. Regulatory Flexibility Act
The Regulatory Flexibility Act (RFA) of 1980 requires the
identification of potentially adverse impacts of Federal
regulations upon small business entities. The RFA specifically
requires the completion of an analysis in those instances where
6
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small business impacts are possible. This rulemaking does not
impose emission measurement requirements beyond those specified
in the current regulations, nor does it change any emission
standard. Because this rulemaking imposes no adverse economic
impacts, an analysis has not been conducted.
Pursuant to the provision of 5 U.S.C. 605(b), I hereby
certify that the promulgated rule will not have an impact on
small entities because no additional costs will be incurred.
E. Paperwork Reduction Act
This rule does not change any information collection
requirements subject to Office of Management and Budget review
under the Paperwork Reduction Act of 1980, 44 U.S.C. 3501 et seq.
F. Statutory Authority
The statutory authority for this proposal is provided by
sections 111 and 301(a) of the Clean Air Act, as amended: 42
U.S.C., 7411 and 7601(a).
LIST OF SUBJECTS
Air pollution control, municipal waste combustors,
polychorinated dibenzo-p-dioxins, sources.
-------
Date The Administrator
It is proposed that 40 CFR Part 60 be amended as follows:
1. The authority citation for Part 60 continues to read as
follows: Authority: Clean Air Act (42 U.S.C. 7401 [et seq.], as
amended by Pub. L 101-549).
2. Replace test Method 23 of Appendix A, with the
following:
Method 23 - Determination of Polychlorinated Dibenzo-p-dioxins
and Polychlorinated Dibenzofurans from Municipal Waste Combustors
1. APPLICABILITY AND PRINCIPLE
1.1 Applicability. This method is applicable to the
determination of emissions of polychlorinated dibenzo-p-dioxins
(PCDD's) and polychlorinated dibenzofurans (PCDF's) from
municipal waste combustors. Calibration standards are selected
for regulated emission levels for municipal waste combustors.
1.2 Principle. A sample is withdrawn isokinetically from the
gas stream and collected in the sample probe, on a glass fiber
filter, and on a packed column of adsorbent material. The sample
cannot be separated into a particle and vapor fraction. The
PCDD's and PCDF's are extracted from the sample, separated by
high resolution gas chromatography (HRGC) , and measured by high
-------
resolution mass spectrometry (HRMS).
2. APPARATUS
2.1 Sampling. A schematic of the sampling train is shown in
Figure 23-1. Sealing greases shall not be used in assembling the
train. The train is identical to that described in Section 2.1
of Method 5 of this appendix with the following additions:
-------
•tack win
GaiFkjw
temperature
eeneor
heated glatl liner
£_ ,_
1
hea
ri
i_i
d
>
tamparatur*
filter
holder
tompvratura
xnior
•8'typa
pilot
g» *xlt
vacuum pump
Figure 23.1 Sampling Train
10
-------
II
-------
2.1.1 Nozzle. The nozzle shall be made of nickel, nickel-
plated stainless steel, quartz, or borosilicate glass.
2.1.2 Sample Transfer Lines. The sample transfer lines, if
needed, shall be heat traced, heavy walled TFE (1/2 in. OD with
1/8 in. wall) with connecting fittings that are capable of
forming leak-free, vacuum-tight connections without using sealing
greases. The line shall be as short as possible and must be
maintained at .>120°C.
2.1.1 Filter Support. Teflon or Teflon-coated wire.
2.1.2 Condenser. Glass, coil type with compatible fittings.
A schematic diagram is shown in Figure 23-2.
2.1.3 Water Bath. Thermostatically controlled to maintain the
gas temperature exiting the condenser at ^20°C (68°F).
2.1.4 Adsorbent Module. Glass container to hold up to 40
grams of resin adsorbent. A schematic diagram is shown in Figure
23-2. Other physical configurations of the water-jacketed resin
trap/condenser assembly are acceptable. The connecting fittings
shall form leak-free, vacuum tight seals. A coarse glass frit is
included to retain the adsorbent in the water-jacketed sorbent
module.
2.1.5 Probe Liner. The probe liner shall be made of glass and
a Teflon ferrule or Teflon coated 0-ring shall be used to make
the seal at the nozzle end of the probe.
12
-------
2.2 Sample Recovery.
2.2.1 Fitting Caps. Ground glass, Teflon tape, or aluminum
foil (Section 2.2.6) to cap off the sample exposed sections of
the train and sorbent module.
2.2.2 Wash Bottles. Teflon, 500-mL.
13
-------
to
o
Flue
Gas
Flow
o
o
* 20/15
o
O
«
w
5
E
E
Sorbent Trap
Glass Sintered Disk
XAD-2
Water Jacket
Glass Wool Plug
Condenser
Cooling Coil
Water Jacket
#20/15
Figure 23.2 Condenser and Adsorbent Trap
14
-------
15
-------
2.2.3 Probe Liner, Probe Nozzle, and Filter Holder Brushes.
Inert bristle brushes with precleaned stainless steel or Teflon
handles. The probe brush shall have extensions of stainless
steel or Teflon, at least as long as the probe. The brushes
shall be properly sized and shaped to brush out the nozzle, probe
liner, and transfer line, if used.
2.2.4 Filter Storage Container. Sealed filter holder, wide-
mouth amber glass jar with Teflon-lined cap, glass petri dish, or
Teflon baggie.
2:2.5 Balance. Triple beam.
2.2.6 Aluminum Foil. Heavy duty, hexane-rinsed (Do not use to
wrap or ship filter samples, because it may react with
particulate matter).
2.2.7 Metal Storage Container. Air tight container to store
silica gel.
2.2.8 Graduated Cylinder. Glass, 250-mL with 2-mL
graduations.
2.2.9 Glass Sample Storage Containers. Amber glass bottles
for sample glassware washes, 500- or 1000-mL, with leak free
Teflon-lined caps.
2.3 Analysis.
2.3.1 Sample Containers. 125- and 250-mL flint glass bottles
with Teflon-lined caps.
16
-------
2.3.2 Test Tubes. Glass.
2.3.3 Soxhlet Extraction Apparatus. Capable of holding 43 x
123 mm extraction thimbles.
2.3.4 Extraction Thimble. Glass, precleaned cellulosic, or
glass fiber.
2.3.5 Pasteur Pipettes. For preparing liquid chromatographic
columns.
2.3.6 Reacti-vials. Amber glass, 2-mL.
2.3.7 Rotary Evaporator. Buchi/Brinkman RF-121 or equivalent.
2*. 3.8 Kuderna-Danish Concentrator Apparatus.
2.3.9 Nitrogen Evaporative Concentrator. N-Evap Analytical
Evaporator Model III or equivalent.
2.3.10 Separatory Funnels. Glass, 2-liter.
2.3.11 Gas Chromatograph. Consisting of the following
components:
2.3.11.1 Oven. Capable of maintaining the separation column
at the proper operating temperature ±10°C and performing
programmed increases in temperature at rates of at least
40°C/min.
2.3.11.2 Temperature Gauges. To monitor column oven,
detector, and exhaust temperatures ±1°C.
2.3.11.3 Flow Systems. Gas metering system to measure sample,
fuel, combustion gas, and carrier gas flows.
17
-------
2.3.11.4 Capillary Columns. A fused silica column,
60 x 0.25 mm inside diameter (ID), coated with DB-5 and a fused
silica column, 30 m x 0.25 mm ID coated with DB-225. Other
column systems may be substituted provided that the user is able
to demonstrate, using calibration and performance checks, that
the column system is able to meet the specifications of Section
6.1.2.2.
2.3.12 Mass Spectrometer. Capable of routine operation at a
resolution of 1:10000 with a stability of ±5 ppm.
2*3.13 Data System. Compatible with the mass spectrometer and
capable of monitoring at least five groups of 25 ions.
2.3.14 Analytical Balance. To measure within 0.1 mg.
3. REAGENTS
3.1 Sampling.
3.1.1 Filters. Glass fiber filters, without organic binder,
exhibiting at least 99.95 percent efficiency (<0.05 percent
penetration) on 0.3-micron dioctyl phthalate smoke particles.
The filter efficiency test shall be conducted in accordance with
ASTM Standard Method D 2986-71 (Reapproved 1978) (incorporated by
reference - see §60.17).
3.1.1.1 Precleaning. All filters shall be cleaned before
their initial use. Place a glass extraction thimble and 1 g of
silica gel and a plug of glass wool into a Soxhlet apparatus,
18
-------
charge the apparatus with toluene, and reflux for a minimum of 3
hours. Remove the toluene and discard it, but retain the silica
gel. Place no more than 50 filters in the thimble onto the
silica gel bed and top with the cleaned glass wool. Charge the
Soxhlet with toluene and reflux for 16 hours. After extraction,
allow the Soxhlet to cool, remove the filters, and dry them under
a clean nitrogen (N2) stream. Store the filters in a glass petri
dishes and seal with Teflon tape.
3.1.2 Adsorbent Resin. Amberlite XAD-2 resin. Thoroughly
cleaned before initial use. Do not reuse resin. If precleaned
XAD-2 resin is purchased from the manufacturer, the cleaning
procedure described in Section 3.1.2.1 is not required.
3.1.2.1 Cleaning. Procedure may be carried out in a giant
Soxhlet extractor. An all-glass filter thimble containing an
extra-coarse frit is used for extraction of XAD-2. The frit is
recessed 10-15 mm above a crenelated ring at the bottom of the
thimble to facilitate drainage. The resin must be carefully
retained in the extractor cup with a glass wool plug and a
stainless steel ring because it floats on methylene chloride.
This process involves sequential extraction in the following
order.
Solvent Procedure
Water Initial Rinse: Place resin in a beaker,
19
-------
rinse once with HPLC water, and discard
water. Refill beaker with water, let
stand overnight, and discard water.
Water Extract with HPLC water for 8 hours.
Methanol Extract with methanol for 22 hours.
Methylene Chloride Extract with methylene chloride for 22
hours.
Methylene Chloride Extract with methylene chloride for 22
hours.
3 v1.2.2 Drying.
3.1.2.2.1 Drying Column. Pyrex pipe, 10.2 cm ID by 0.6 m
long, with suitable retainers.
3.1.2.2.2 Procedure. The adsorbent must be dried with clean
inert gas. Liquid nitrogen from a standard commercial liquid
nitrogen cylinder has proven to be a reliable source for large
volumes of gas free from organic contaminants. Connect the
liquid nitrogen cylinder to the column by a length of cleaned
copper tubing, 0.95 cm ID, coiled to pass through a heat source.
A convenient heat source is a water-bath heated from a steam
line. The final nitrogen temperature should only be warm to the
touch and not over 40°C. Continue flowing nitrogen through the
adsorbent until all the residual solvent is removed. The flow
rate should be sufficient to gently agitate the particles, but
20
-------
not so excessive as to cause the particles to fracture.
3.1.2.3 Quality Control Check. The adsorbent must be checked
for residual methylene chloride (MeCl2) as well as PCDDs and
PCDFs prior to use. The analyst may opt to omit this check for
precleaned XAD-2.
3.1.2.3.1 MeCl2 Residue Extraction. Weigh a 1.0 g sample of
dried resin into a small vial, add 3 mL of toluene, cap the vial,
and shake it well.
3.1.2.3.2 MeCl2 Residue Analysis. Inject a 2 /xl sample of the
extract into a gas chromatograph operated under the following
conditions:
Column: 6 ft x 1/8 in stainless steel containing 10 percent
OV-101™ on 100/120 Supelcoport.
Carrier Gas: Helium at a rate of 30 mL/min.
Detector: Flame ionization detector operated at a sensitivity
of 4 x 10-11 A/mV.
Injection Port Temperature: 250°C.
Detector Temperature: 305°C.
Oven Temperature: 30°C for 4 min; programmed to rise at
40°C/min until it reaches 250°C; return to 30°C after 17
minutes.
Compare the results of the analysis to the results from the
reference solution. Prepare the reference solution by injecting
21
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4.0 /il of methylene chloride into 100 mL of toluene. This
corresponds to 100 /xg of methylene chloride per g of adsorbent.
The maximum acceptable concentration is 1000 /ig/g of adsorbent.
If the adsorbent exceeds this level, drying must be continued
until the excess methylene chloride is removed.
3.1.2.3.3 PCDD and PCDF Check. Extract the adsorbent sample
as described in Section 5.1. Analyze the extract as described in
Section 5.3. If any of the PCDDs or PCDFs (tetra through hexa)
are present at concentrations above the target detection limits
(TDLs), the adsorbent must be recleaned by repeating the last
step of the cleaning procedure. The TDLs for the various
PCDD/PCDF congeners are listed in Table 1.
3.1.2.4 Storage. After cleaning, the adsorbent may be stored
in a wide mouth amber glass container with a Teflon-lined cap or
placed in glass adsorbent modules tightly sealed with glass
stoppers. It must be used within 4 weeks of cleaning. If
precleaned adsorbent is purchased in sealed containers, it must
be used within 4 weeks after the seal is broken.
3.1.3 Glass Wool. Cleaned by sequential immersion in three
aliquots of methylene chloride, dried in a 110°C oven, and stored
in a methylene chloride-washed glass container with a Teflon-
lined screw cap.
3.1.4 Water. Deionized distilled and stored in a methylene
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chloride-rinsed glass container with a Teflon-lined screw cap.
3.1.5 Silica Gel. Indicating type, 6 to 16 mesh. If
previously used, dry at 175° C (350°F) for two hours. New silica
gel may be used as received. Alternatively, other types of
desiccants (equivalent or better) may be used, subject to the
approval of the Administrator.
3.1.6 Chromic Acid Cleaning Solution. Dissolve 20 g of sodium
dichromate in 15 mL of water, and then carefully add 400 mL of
concentrated sulfuric acid.
3'. 1.7 HPLC Water.
3.2 Sample Recovery.
3.2.1 Acetone. Pesticide quality.
3.2.2 Toluene. Pesticide quality.
3.3 Analysis.
3.3.1 Potassium Hydroxide. ACS grade, 2-percent
(weight/volume) in water.
3.3.2 Sodium Sulfate. Granulated, reagent grade. Purify
prior to use by rinsing with methylene chloride and oven drying.
Store the cleaned material in a glass container with a Teflon-
lined screw cap.
3.3.3 Sulfuric Acid. Reagent grade.
3.3.4 Sodium Hydroxide. l.O N. Weigh 40 g of sodium hydroxide
into a 1-liter volumetric flask. Dilute to 1 liter with water.
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3.3.5 Hexane. Pesticide grade.
3.3.6 Methy1ene Chloride. Pesticide grade.
3.3.7 Benzene. Pesticide grade.
3.3.8 Ethyl Acetate.
3.3.9 Methanol. Pesticide grade.
3.3.10 Toluene. Pesticide grade.
3.3.11 Nonane. Pesticide grade.
3.3.12 Cyclohexane. Pesticide Grade.
3.3.13 Basic Alumina. Activity grade 1, 100-200 mesh. Prior
to use, activate the alumina by heating for 16 hours at 130°C.
Store in a desiccator. Pre-activated alumina may be purchased
from a supplier and may be used as received.
3.3.14 Silica Gel. Bio-Sil A, 100-200 mesh. Prior to use,
activate the silica gel by heating for at least 30 minutes at
180°C. After cooling, rinse the silica gel sequentially with
methanol and methylene chloride. Heat the rinsed silica gel at
50°C for 10 minutes, then increase the temperature gradually to
180°C over 25 minutes and maintain it at this temperature for
90 minutes. Cool at room temperature and store in a glass
container with a Teflon-lined screw cap.
3.3.15 Silica Gel Impregnated with Sulfuric Acid. Combine 100
g of silica gel with 44 g of concentrated sulfuric acid in a
screw capped glass bottle and agitate thoroughly. Disperse the
24
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solids with a stirring rod until a uniform mixture is obtained.
Store the mixture in a glass container with a Teflon-lined screw
cap.
3.3.16 Silica Gel Impregnated with Sodium Hydroxide. Combine
39 g of 1 N sodium hydroxide with 100 g of silica gel in a screw
capped glass bottle and agitate thoroughly. Disperse solids with
a stirring rod until a uniform mixture is obtained. Store the
mixture in glass container with a Teflon-lined screw cap.
3.3.17 Carbon/Celite. Combine 10.7 g of AX-21 carbon with 124
g of Celite 545 in a 250-mL glass bottle with a Teflon-lined
screw cap. Agitate the mixture thoroughly until a uniform
mixture is obtained. Store in the glass container.
3.3.18 Nitrogen. Ultra high purity.
3.3.19 Hydrogen. Ultra high purity.
3.3.20 Internal Standard Solution. Prepare a stock standard
solution containing the isotopically labelled PCDD's and PCDF's
at the concentrations shown in Table 2 under the heading
"Internal Standards" in 10 mL of nonane.
3.3.21 Surrogate Standard Solution. Prepare a stock standard
solution containing the isotopically labelled PCDD's and PCDF's
at the concentrations shown in Table 2 under the heading
"Surrogate Standards" in 10 mL of nonane.
3.3.22 Recovery Standard Solution. Prepare a stock standard
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solution containing the isotopically labelled PCDD's and PCDF's
at the concentrations shown in Table 2 under the heading
"Recovery Standards" in 10 mL of nonane.
4. PROCEDURE
4.1 Sampling. The complexity of this method is such that, in
order to obtain reliable results, testers and analysts should be
trained and experienced with the procedures.
4.1.1 Pretest Preparation.
4.1.1.1 Cleaning Glassware. All gjLass components of the train
upstream of and including the adsorbent module, shall be cleaned
as described in Section 3A of the "Manual of Analytical Methods
for the Analysis of Pesticides in Human and Environmental
Samples." Special care shall be devoted to the removal of
residual silicone grease sealants on ground glass connections of
used glassware. Any residue shall be removed by soaking the
glassware for several hours in a chromic acid cleaning solution
prior to cleaning as described above.
4.1.1.2 Adsorbent Trap. The traps shall be loaded in a clean
area to avoid contamination. They may not be loaded in the
field. Fill a trap with 20 to 40 g of XAD-2. Follow the XAD-2
with glass wool and tightly cap both ends of the trap. Add 40 /zl
of the surrogate standard solution (Section 3.3.21) to each trap
for a sample that will be split prior to analysis or 20 fj.1 of the
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surrogate standard solution (Section 3.3.21) to each trap for
samples that will not be split for analysis (Section 5.1). After
addition of the surrogate standard solution, the trap must be
used within 14 days. Keep the spiked sorbent under refrigeration
until use.
4.1.1.3 Sampling Train. It is suggested that all components
be maintained according to the procedure described in APTD-0576.
4.1.1.4 Silica Gel. Weigh several 200 to 300 g portions of
silica gel in air tight containers to the nearest 0.5 g. Record
the.total weight of the silica gel plus container, on each
container. As an alternative, the silica gel may be weighed
directly in the fifth impinger just prior to sampling.
4.1.1.5 Filter. Check each filter against light for
irregularities and flaws or pinhole leaks. Pack the filters flat
in a clean glass container or Teflon baggie. Do not mark filter
with ink or any other contaminating substance.
4.1.2 Preliminary Determinations. Same as Section 4.1.2
Method 5.
4.1.3 Preparation of Sampling Train.
4.1.3.1 During preparation and assembly of the sampling train,
keep all train openings where contamination can enter, sealed
until sampling is about to begin. Wrap sorbent module with
aluminum foil to shield from radiant heat of sun light. (NOTE:
27
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Do not use sealant grease in assembling the train.)
4.1.3.2 Place approximately 100 mL of water in the second and
third impingers, leave the first and fourth impingers empty, and
transfer approximately 200 to 300 g of preweighed silica gel from
its container to the fifth impinger.
4.1.3.3 Place the silica gel container in a clean place for
later use in the sample recovery. Alternatively, the weight of
the silica gel plus the fifth impinger may be determined to the
nearest 0.5 g and recorded.
4*1.3.4 Assemble the sampling train as shown in Figure 23-1.
4.1.3.5 Turn on the adsorbent module and condenser coil
recirculating pump and begin monitoring the adsorbent module gas
entry temperature. Ensure proper sorbent gas entry temperature
before proceeding and before sampling is initiated. It is
extremely important that the XAD-2 adsorbent resin temperature
never exceed 50°C because thermal decomposition and breakthrough
of surrogate standards will occur. During testing, the XAD-2
temperature must not exceed 20°C for efficient capture of the
PCDD's and PCDF's.
4.1.4 Leak-Check Procedure. Same as Method 5, Section 4.1.4.
4.1.5 Sampling Train Operation. Same as Method 5,
Section 4.1.5.
4.2 Sample Recovery. Proper cleanup procedure begins as soon
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as the probe is removed from the stack at the end of the sampling
period. Seal the nozzle end of the sampling probe with Teflon
tape or aluminum foil.
When the probe can be safely handled, wipe off all external
particulate matter near the tip of the probe. Remove the probe
from the train and close off both ends with aluminum foil. Seal
off the inlet to the train with Teflon tape, a ground glass cap,
or aluminum foil.
Transfer the probe and impinger assembly to the cleanup area.
This area shall be clean and enclosed so that the chances of
losing or contaminating the sample are minimized. Smoking, which
could contaminate the sample, shall not be allowed in the cleanup
area. Cleanup personnel shall wash their hands prior to sample
recovery.
Inspect the train prior to and during disassembly and note any
abnormal conditions, e.g., broken filters, colored impinger
liquid, etc. Treat the samples as follows:
4.2.1 Container No. 1. Either seal the filter holder or
carefully remove the filter from the filter holder and place it
in its identified container. Do not place the filter in aluminum
foil. Use a pair of cleaned tweezers to handle the filter. If
it is necessary to fold the filter, do so such that the
particulate cake is inside the fold. Carefully transfer to the
29
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container any particulate matter and filter fibers which adhere
to the filter holder gasket, by using a dry inert bristle brush
and a sharp-edged blade. Seal the container with Teflon tape.
4.2.2 Adsorbent Module. Remove the module from the train,
tightly cap both ends, label it, and store it on ice for
transport to the laboratory.
4.2.3 Container No. 2. Quantitatively recover material
deposited in the nozzle, probe transfer lines, the front half of
the filter holder, and the cyclone, if used, first, by brushing
while rinsing three times with acetone and then, by rinsing the
probe three times with toluene. Collect all the rinses in
Container No. 2.
Rinse the back half of the filter holder three times with
acetone. Rinse the connecting line between the filter and the
condenser three times with acetone. Soak the connecting line
with three separate portions of toluene for 5 minutes each. If
using a separate condenser and adsorbent trap, rinse the
condenser in the same manner as the connecting line. Collect all
the rinses in Container No. 2 and mark the level of the liquid on
the container.
4.2.4 Impinger Water. Measure the liquid in the first four
impingers to within 1 mL by using a graduated cylinder or by
weighing it to within 0.5 g by using a balance. Record the
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volume or weight of liquid present. This information is required
to calculate the moisture content of the effluent gas. Discard
the liquid after measuring and recording the volume or weight.
4.2.5 Silica Gel. Note the color of the indicating silica gel
to determine if it has been completely spent and make a mention
of its condition. Transfer the silica gel from the fifth
impinger to its original container and seal.
5. ANALYSIS
All glassware shall be cleaned as described in Section 3A of
the."Manual of Analytical Methods for the Analysis of Pesticides
in Human and Environmental Samples." All samples must be
extracted within 30 days of collection and analyzed within 45
days of extraction.
5.1 Sample Extraction. The analyst may choose to split the
sample extract after the completion of sample extraction
procedures. One half of the sample can then be archived. Sample
preparation procedures are given for using the entire sample and
for splitting the sample.
5.1.1 Extraction System. Place an extraction thimble (Section
2.3.4), 1 g of silica gel, and a plug of glass wool into the
Soxhlet apparatus, charge the apparatus with toluene, and reflux
for a minimum of 3 hours. Remove the toluene and discard it, but
retain the silica gel. Remove the extraction thimble from the
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extraction system and place it in a glass beaker to catch the
solvent rinses.
5.1.2 Container No. 1 (Filter). Transfer the contents
directly to the glass thimble of the extraction system and
extract them simultaneously with the XAD-2 resin.
5.1.3 Adsorbent Cartridge. Suspend the adsorbent module
directly over the extraction thimble in the beaker (See Section
5.1.1). The glass frit of the module should be in the up
position. Using a Teflon squeeze bottle containing toluene,
flush the XAD-2 into the thimble onto the bed of cleaned silica
gel. Thoroughly rinse the glass module catching the rinsings in
the beaker containing the thimble. If the resin is wet,
effective extraction can be accomplished by loosely packing the
resin in the thimble. Add the XAD-2 glass wool plug to the
thimble.
5.1.4 Container No. 2 (Acetone and Toluene). Concentrate the
sample to a volume of about 1-2 mL using a Kuderna-Danish
concentrator apparatus, followed by N2 blow down at a temperature
of less than 37°C. Rinse the sample container three times with
small portions of methylene chloride and add these to the
concentrated solution and concentrate further to near dryness.
This residue contains particulate matter removed in the rinse of
the sampling train probe and nozzle. Add the concentrate to the
32
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filter and the XAD-2 resin in the Soxhlet apparatus described in
Section 5.1.1.
5.1.5 Extraction. For samples that are to be split prior to
analysis add 40 /il of the internal standard solution
(Section 3.3.20) to the extraction thimble containing the
contents of the adsorbent cartridge, the contents of
Container No. 1, and the concentrate from Section 5.1.4.
Alternatively, 20 /xl of the internal standard solution
(Section 3.3.20) for samples that are not to be split prior to
analysis. Cover the contents of the extraction thimble with the
cleaned glass wool plug to prevent the XAD-2 resin from floating
into the solvent reservoir of the extractor. Place the thimble
in the extractor, and add the toluene contained in the beaker to
the solvent reservoir. Add additional toluene to fill the
reservoir approximately 2/3 full. Add Teflon boiling chips and,
assemble the apparatus. Adjust the heat source to cause the
extractor to cycle three times per hour. Extract the sample for
16 hours. After extraction, allow the Soxhlet to cool. Transfer
the toluene extract and three 10-mL rinses to the rotary
evaporator. Concentrate the extract to approximately 10 mL. If
decided to split the sample, store one half for future use, and
analyze the other half according to the procedures in Sections
5.2 and 5.3. In either case, use a nitrogen evaporative
33
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concentrator to reduce the volume of the sample being analyzed to
near dryness. Dissolve the residue in 5 mL of hexane.
5.2 Sample Cleanup and Fractionation.
The following sample cleanup and fractionation procedures are
recommended. Alternative procedures may be utilized providing
acceptable identification criteria (Section 5.3.2.5) and
quantification criteria (Section 5.3.2.6) are met.
5.2.1 Silica Gel Column. Pack one end of a glass column,
20 mm x 230 mm, with glass wool. Add in sequence, 1 g silica
gel/ 2 g of sodium hydroxide impregnated silica gel, 1 g silica
gel, 4 g of acid-modified silica gel, and 1 g of silica gel.
Wash the column with 30 mL of hexane and discard. Add the sample
extract, dissolved in 5 mL of hexane to the column with two
additional 5-mL rinses. Elute the column with an additional 90
mL of hexane and retain the entire eluate. Concentrate this
solution to a volume of about 1 mL using the nitrogen evaporative
concentrator (Section 2.3.9).
5.2.2 Basic Alumina Column. Shorten a 25-mL disposable
Pasteur pipette to about 16 mL. Pack the lower section with
glass wool and 12 g of basic alumina. Transfer the concentrated
extract from the silica gel column to the top of the basic
alumina column and elute the column sequentially with 120 mL of
0.5 percent methylene chloride in hexane followed by 120 mL of 35
34
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percent methylene chloride in hexane. Discard the first 120 raL
of eluate. Collect the second 120 raL of eluate and concentrate
it to about 0.5 mL using the nitrogen evaporative concentrator.
Transfer this extract with hexane to "13 mL tubes".
5.2.3 AX-21 Carbon/Celite 545 Column. Remove the bottom 0.5
in. from the tip of a 2-mL disposable Pasteur pipette. Insert a
glass fiber filter disk or glass wool plug in the top of the
pipette 2.5 cm from the constriction. Add sufficient
carbon/Celite™ mixture to form a 2 cm column (the 0.6 mL mark
column. Top with a glass wool plug. In some cases AX-21 carbon
fines may wash through the glass wool plug and enter the sample.
This may be prevented by adding a celite plug to the exit end of
the column. Pre-elute the column with 5 mL toluene, followed by 1
mL of a 50:50 methylene chloride/cyclohexane mixture, followed by
5 mL of hexane. Load in sequence, the sample extract in 1 mL
hexane, 2x0.5 mL rinses in hexane, 2 mL of 50 percent methylene
chloride in hexane and 2 mL of 50 percent benzene in ethyl
acetate and discard the eluates. Invert the column and elute in
the reverse direction with 13 mL of toluene. Collect this
eluate. Concentrate the eluate in a nitrogen evaporator at 45°C
to about 1 mL. Transfer the concentrate to a Reacti-vial using a
toluene rinses and concentrate to near dryness (less than 20
using a stream of N2. Store extracts at room temperature,
35
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shielded from light, until the analysis is performed.
5.3 Analysis. Analyze the sample with a gas chromatograph
coupled to a mass spectrometer (GC/MS) using the instrumental
parameters in Sections 5.3.1 and 5.3.2. Immediately prior to
analysis, add a 20 pil aliquot of the recovery standard solution
from Table 2 to each sample. A 2 /il aliquot of the extract is
injected into the GC. Sample extracts are first analyzed using
the DB-5 capillary column to determine the concentration of each
isomer of PCDD's and PCDF's (tetra-through octa-). If 2,3,7,8-
TCDF is detected in this analysis, then analyze another aliquot
of the sample in a separate run, using the DB-225 column to
measure the 2,3,7,8 tetra-chloro dibenzofuran isomer. Other
column systems may be used, provided that it can be demonstrated
using calibration and performance checks that the column system
is able to meet the specifications of Section 6.1.2.
5.3.1 Gas Chromatograph Operating Conditions. The recommended
conditions are shown in Table 4.
5.3.2 High Resolution Mass Spectrometer.
5.3.2.1 Resolution. 10,000 resolving power or 100 ppm
mass/mass.
5.3.2.2 lonization Mode. Electron impact.
5.3.2.3 Source Temperature 250°C.
5.3.2.4 Monitoring Mode. Selected ion monitoring. A list of
36
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the various ions to be monitored is presented in Table 5.
5.3.2.5 Identification Criteria. The following identification
criteria shall be used for the characterization of
polychlorinated dibenzodioxins and dibenzofurans.
1. The integrated ion-abundance ratio (M/M+2 or M+2/M+4) shall
be within 15 percent of the theoretical value. The acceptable
ion-abundance ratio ranges (±15%) for the identification of
chlorine-containing compounds are given in Table 6. If the ion-
abundance ratio ranges are the outside those in Table 6, the
source has the option of using the results if the concentration
is determined using procedures in Section 9.3 or redoing the
analysis to eliminate the unacceptable ion-abundance ratio.
2. The retention time for the analytes must be within 3
seconds of the corresponding 13C-labeled internal standard or
surrogate standard.
3. The monitored ions, shown in Table 5 for a given analyte,
shall reach their maximum within 2 seconds of each other.
4. The identification of specific isomers that do not have
corresponding 13C-labeled standards is done by comparison of the
relative retention time (RRT) of the analyte to the nearest
internal standard retention time with reference (i.e., within
0.005 RRT units) to the comparable RRT's found in the continuing
calibration.
37
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5. The signal to noise ratio for all monitored ions must be
greater than 2.5.
6. The confirmation of 2, 3, 7, 8-TCDF shall satisfy all of
the above identification criteria.
7. Any PCDF coeluting (±2 s) with a peak in the corresponding
PCDPE channel, of intensity 10% or greater compared to the
analyte peak is evidence of a positive interference, the source
may opt keep the value to calculate CDD/CDF concentration or
conduct a complete reanalysis in an effort to remove or shift the
interference. If a reanalysis is conducted, all values from the
reanalyzed sample will be used for CDD/CDF concentration
calculations.
8. Set the mass spectrometer lock channels as specified in
Table 5. Monitor the quality control check channels specified in
Table 5 to verify instrument stability during the analysis. If
the signal varies by more than 25 percent from the average
response, results for all isomers at corresponding residence time
shall be invalid. The source has the options of conducting
additional cleanup procedures on the other portion of the sample
for split samples or diluting the original sample or following
other procedures recommended by the Administrator. When a
complete reanalysis is conducted, all concentration calculations
shall be based on the reanalyzed sample.
38
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5.3.2.6 Quantification. The peak areas for the two ions
monitored for each analyte are summed to yield the total response
for each analyte. Each internal standard is used to quantify the
indigenous PCDD's or PCDF's in its homologous series. For
example, the 13C12-2, 3 , 7, 8-tetra chlorinated dibenzodioxin is used
to calculate the concentrations of all other tetra chlorinated
isomers. Recoveries of the tetra- and penta- internal standards
are calculated using the 13C12-1,2,3,4-TCDD. Recoveries of the
hexa- through octa- internal standards are calculated using 13C12-
1,2;3,7,8,9-HxCDD. Recoveries of the surrogate standards are
calculated using the corresponding homolog from the internal
standard. When no peak is detected, the noise level, as measured
by the intensity of the noise in a clear zone of the
chromatogram, is used to calculate the detection limit. Tables
7, 8, and 9 summarize the quantification relationships for the
unlabeled analytes, internal standards and surrogate standards,
respectively.
6. CALIBRATION
Same as Method 5 with the following additions.
6.1 GC/MS System.
6.1.1 Initial Calibration. Calibrate the GC/MS system using
the set of five standards shown in Table 3. The relative
standard deviation for the mean response factor from each of the
39
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unlabeled analytes (Table 3) and of the internal and surrogate
standards shall be less than or equal to the values in Table 6.
The signal to noise ratio for the GC signal present in every
selected ion current profile shall be greater than or equal to
10. The ion abundance ratios shall be within the control limits
in Table 5.
6.1.2 Daily Performance Check.
6.1.2.1 Calibration Check. Inject 2 /il of solution Number 3
from Table 3. Calculate the relative response factor (RRF) for
each compound and compare each RRF to the corresponding mean RRF
obtained during the initial calibration. The analyzer
performance is acceptable if the measured RRF's for the labeled
and unlabeled compounds for the daily run are within the limits
of the mean values shown in Table 10. In addition, the ion-
abundance ratios shall be within the allowable control limits
shown in Table 6.
6.1.2.2 Column Separation Check. Inject 2 /ul of a solution of
a mixture of PCDD's and PCDF's that documents resolution between
2,3,7,8-TCDD and other TCDD isomers. Resolution is defined as a
valley between peaks that is less than 25 percent of the lower of
the two peaks. Identify and record the retention time windows
for each homologous series. Perform a similar resolution check
on the confirmation column to document the resolution between
40
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2,3,7,8 TCDF and other TCDF isomers.
6.2 Lock Channels. Set mass spectrometer lock channels as
specified in Table 5. Monitor the quality control check channels
specified in Table 5 to verify instrument stability during the
analysis.
7. QUALITY CONTROL
7.1 Sampling Train Collection Efficiency Check. Add 40 ptl of
the surrogate standards in Table 2 for samples split for analysis
or 20 /zl of the surrogate standards for sample not split for
analysis to the adsorbent cartridge of each train before
collecting the field samples.
7.2 Internal Standard Percent Recoveries. A group of nine
carbon-labeled PCDDs and PCDFs representing the tetra- through
octachlorinated homologues, is added to every sample prior to
extraction. The role of the internal standards is to quantify
the native PCDD's and PCDF's present in the sample as well as to
determine the overall method efficiency. Recoveries of the
internal standards shall be between 40 to 130 percent for the
tetra- through hexachlorinated compounds while the range is 25 to
130 percent for the hepta- and octachlorinated homologues.
7.3 Surrogate Standard Recoveries. The five surrogate
compounds in Table 3 are added to the resin in the adsorbent
sampling cartridge before the sample is collected. The surrogate
41
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recoveries are measured relative to the internal standards and
are a measure of the sampling train collection efficiency. They
are not used to measure the native PCDD's and PCDF's. All
surrogate standard recoveries shall be between 70 and
130 percent. Poor recoveries for all the surrogates may be an
indication of breakthrough in the sampling train. If the
recovery of all standards is below 70 percent, the sampling runs
must be repeated. As an alternative, the sampling runs do not
have to be repeated if the final results are divided by the
fraction of surrogate recovery (on a homolog group basis) . Poor
recoveries of isolated surrogate compounds should not be grounds
for rejecting an entire set of samples.
7.4 Toluene QA Rinse. Report the results of the toluene QA
rinse separately from the total sample catch. Do not add it to
the total sample.
7.5 Detection Limits. Calculate the'detection limits using
the equation in Section 9.8. If the detection limits meet the
Target Detection Limits (TDLs) in Table 1, then they are
considered acceptable. If the TDLs are not met, the impact of
the detection limits shall be calculated using the procedures in
Section 9.9. If the maximum potential value of the sum of the
summed detection limits is less then 50 percent of the emission
standard, the detection limits are acceptable. If the value is
42
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greater than 50 percent of the emission standard, then the
analysis and/or sampling and analysis must be repeated until
acceptable detection limits are obtained.
8. QUALITY ASSURANCE
8.1 Applicability. When the method is used to analyze samples
to demonstrate compliance with a source emission regulation, an
audit sample must be analyzed, subject to availability.
8.2 Audit Procedure. Analyze an audit sample with each set of
compliance samples. The audit sample contains tetra through octa
isomers of PCDD and PCDF. Concurrently analyze the audit sample
and a set of compliance samples in the same manner to evaluate
the technique of the analyst and the standards preparation. The
same analyst, analytical reagents, and analytical system shall be
used both for the compliance samples and the EPA audit sample.
8.3 Audit Sample Availability. Audit samples will be supplied
only to enforcement agencies for compliance tests. Audit samples
may be obtained by writing:
Source Test Audit Coordinator (MD-77B)
Quality Assurance Division
Atmospheric Research and Exposure Assessment Laboratory
U.S. Environmental Protection Agency
Research Triangle Park, NC 27711
or by calling the Source Test Audit Coordinator (STAC) at (919)
43
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541-7834. The audit sample request must be made at least 30 days
prior to the scheduled compliance sample analysis.
8.4 Audit Results. Calculate the audit sample concentration
according to the calculation procedure provided in the audit
instructions included with the audit sample. Fill in the audit
sample concentration and the analyst's name on the audit response
form included with the audit instructions. Send one copy to the
EPA Regional Office or the appropriate enforcement agency and a
second copy to the STAC. The EPA Regional office or the
appropriate enforcement agency will report the results of the
audit to the laboratory being audited. Include this response
with the results of the compliance samples in relevant reports to
the EPA Regional Office or the appropriate enforcement agency.
9. CALCULATIONS
Same as Method 5, Section 6 with the following additions.
9.1 Nomenclature.
Aai = Integrated ion current of the noise at the retention time
of the analyte.
Acij = Integrated ion current of the two ions characteristic of
compound i in the jth calibration standard.
A*cij = Integrated ion current of the two ions characteristic of
the internal standard i in the jth calibration standard.
- Integrated ion current of the two ions characteristic of
44
-------
surrogate compound i in the calibration standard.
Ai = Integrated ion current of the two ions characteristic of
compound i in the sample.
A*i = Integrated ion current of the two ions characteristic of
internal standard i in the sample.
Arg = Integrated ion current of the two ions characteristic of
the recovery standard.
Asi = Integrated ion current of the two ions characteristic of
surrogate compound i in the sample.
Ci = Concentration of PCDD or PCDF i in the sample, pg/M3.
CT = Total concentration of PCDD's or PCDF's in the sample,
pg/M3.
DL = Detection limit, pg/sample.
DLhs = Detection limit for each homologous series, pg/sample.
DLsura = Sum of all isomers times the corresponding detection
limit, ng/m3.
Hai = Summed heights of the noise at the retention time of the
analyte in the two analyte channels.
mci = Mass of compound i in the calibration standard injected
into the analyzer, pg.
m*ci = Mass of labeled compound i in the calibration standard
injected into the analyzer, pg.
m*i = Mass of internal standard i added to the sample, pg.
45
-------
mrs = Mass of recovery standard in the calibration standard
injected into the analyzer, pg.
ms = Mass of surrogate compound in the sample to be analyzed,
pg-
msi = Mass of surrogate compound i in the calibration standard,
pg.
RRFi = Relative response factor for compound i.
RRFrs = Recovery standard response factor.
RRFS = Surrogate compound response factor.
Vm(std)= Metered volume of sample run, dscm.
1000 = pg per ng.
9.2 Average Relative Response Factor.
i _B_ A m *
RRF = -£ cij ci Eq. 23-1
1 nj=i A* m
cij ci
9.3 Concentration of the PCDD's and PCDF's.
m1 A
C. = Eq. 23-2
A<* RRF, V
9.4 Recovery Standard Response Factor.
46
-------
Aci m
RRFra = - — Eq. 23-3
9.5 Recovery of Internal Standards (R*)
A, m
_xlOO% Eq. 23-4
I RF
rs rs
9.6 Surrogate Compound Response Factor,
c si
RRFS = - Zi. Eq. 23-5
S
9.7 Recovery of Surrogate Compounds (R.) .
«,<
Rs = ai— xiQO% Eq. 23-6
A^ RRFg mg
9.8 Detection Limit (DL). The detection limit can be
calculated based on either the height of the noise or the area of
47
-------
the noise using one of the two equations.
Detection limit using height for the DB-225 column. Three and
one half times the height has been empirically determined to give
area.
2.5 (3.5 x H .) m,
DL = Eq. 23-7
Detection limit using height for the DB-5 column. Five times the
height has been empirically determined to give area.
2.5 (5 x H .) ml
DL = Eq. 23-8
Detection limit using area of the noise,
2 5 A m
DL = — —- Eq. 23-9
Ac*, RRF.
9.9 Summed Detection Limits. Calculate the maximum potential
value of the summed detection limits. If the isomer (group of
unresolved isomers) was not detected, use the value calculated
for the detection limit in Section 9.8 above. If the isomer
(group of unresolved isomers) was detected, use the value (target
48
-------
detection limit) from Table 1.
DL.um = (13 DLTCDD + l6 DL — + 12
+ 14 DL + 7 D
„
+ 2 DL + 4 DL + DL . 23-10
HpCDD HpCDF OCDD
Note: The number of isomers used to calculate the summed
detection limit represent the total number of isomers typically
separated and not the actual number of isomers for each series.
9.10 Total Concentration of PCDD's and PCDF's in the Sample.
7. Eq. 23-11
Any PCDDs or PCDFs that are reported as not detected (below the
DL) shall be counted as zero for the purpose of calculating the
total concentration of PCDDs and PCDFs in the sample.
10. BIBLIOGRAPHY
1. American Society of Mechanical Engineers. Sampling for the
Determination of Chlorinated Organic Compounds in Stack
Emissions. Prepared for U.S. Department of Energy and U.S.
Environmental Protection Agency. Washington DC. December 1984.
25 p.
2. American Society of Mechanical Engineers. Analytical
49
-------
Procedures to Assay Stack Effluent Samples and Residual
Combustion Products for Polychlorinated Dibenzo-p-Dioxins (PCDD)
and Polychlorinated Dibenzofurans (PCDF). Prepared for the U.S.
Department of Energy and U.S. Environmental Protection Agency.
Washington, DC. December 1984. 23 p.
3. Thompson, J. R. (ed.). Analysis of Pesticide Residues in
Human and Environmental Samples. U.S. Environmental Protection
Agency. Research Triangle Park, NC. 1974.
4. Triangle Laboratories. Case Study: Analysis of Samples
for -the Presence of Tetra Through Octachloro-p-Dibenzodioxins and
Dibenzofurans. Research Triangle Park, NC. 1988. 26 p.
5. U.S. Environmental Protection Agency. Method 8290 - The
Analysis of Polychlorinated Dibenzo-p-dioxin and Polychlorinated
Dibenzofurans by High-Resolution Gas Chromatography/
High-Resolution Mass Spectrometry. In: Test Methods for
Evaluating Solid Waste. Washington, DC. SW-846.
6. Personnel communications with R. L. Harless of U.S. EPA and
Triangle Laboratory staff.
50
-------
TABLE 23-1. TARGET DETECTION LIMITS (TDLs)
ANALYTE
TCDD/TCDF
PeCDD/PeCDF
HxCDD/HxCDF
HpCDD/HpCDF
OCDD/OCDF
TDL (pg/Sample Train)
50
250
250
250
500
TABLE 23-2. COMPOSITION OF THE SAMPLE FORTIFICATION AND RECOVERY
STANDARDS SOLUTIONS*
ANALYTE
CONCENTRATION (pg//xL)
Internal Standards
13C12
13c12
13p
(~12
13c12
13c12
13p
*-12
13c12
13c12
13/-i
(-12
-2,
-1,
-1,
-1,
3,
2,
2,
2,
7,
3,
3,
3,
8
7
6
4
-TCDD
,8
,7
,6
-PeCDD
, 8-HxCDD
, 7,8-HpCDD
-OCDD
-2,
-1,
-1,
-1,
3,
2,
2,
2,
7,
3,
3,
3,
8
7
6
4
-TCDF
,8
,7
,6
-PeCDF
, 8-HxCDF
,7,8-HpCDF
100
100
100
100
100
100
100
100
100
Surrogate Standards
37Cl4-2
13C12
13C12
13C12
13/"i
<~12
-1,
-2,
-1,
-1,
,3,7
2,
3,
2,
2,
3,
4,
3,
3,
,8-TCDD
4
7
4
4
,7
,8
,7
,7
,8-HxCDD
-PeCDF
,8-HxCDF
,8,9-HpCDF
100
100
100
100
100
Recovery Standards
51
-------
13C12-1,2,3,4-TCDD
13C12-1,2,3,7,8, 9-HxCDD
100
100
'Calibration levels are specific for samples at
the MWC compliance standard level.
52
-------
TABLE 23-3. COMPOSITION OF THE INITIAL CALIBRATION SOLUTIONS
COMPOUND
SOLUTION NO.
CONCENTRATIONS (pg//il)
1
2
3
4
5
UNLABELED ANALYTES
2,3,7,8-TCDD
2,3,7,8-TCDF
1,2,3,7,8-PeCDD
1,2,3,7,8-PeCDF
2,3,4,7,8-PeCDF
1,2,3,4,7,8-HxCDD
1,2,3,6,7,8-HxCDD
1,2, 3,7,8, 9-HxCDD
1,2,3,4,7,8-HxCDF
1,2,3,6,7,8-HxCDF
1,2,3,7,8,9-HxCDF
2,3,4,6,7,8-HxCDD
1,2,3,4,6,7,8-HpCDD
1,2,3,4,6,7,8-HpCDF
1,2,3,4,7,8,9-HpCDF
OCDD
OCDF
0.5
0.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
5
5
1
1
5
5
5
5
5
5
5
5
5
5
5
5
5
10
10
5
5
25
25
25
25
25
25
25
25
25
25
25
25
25
50
50
50
50
250
250
250
250
250
250
250
250
250
250
250
250
250
500
500
100
100
500
500
500
500
500
500
500
500
500
500
500
500
500
1000
1000
INTERNAL STANDARDS
13C12-2,3,7,8-TCDD
13C12-l,2,3,7,8-PeCDD
13C12-l,2,3,6,7,8-HxCDD
13C12- 1 ,2,3,4,6,7,8 -HpCDD
13C12-OCDD
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
53
-------
13C12-2,3,7,8-TCDF
13C12-l,2,3,7,8-PeCDF
13C12-l,2,3,6,7,8-HxCDF
13C12-1, 2,3,4, 6,7, 8-HpCDF
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
TABLE 23-3. (Continued)
COMPOUND
SOLUTION NO.
CONCENTRATION (pg/pil)
1
2
3
4
SURROGATE STANDARDS
37Cl4-2,3,7,8-TCDD
13C12-2/3,4/7,8-PeCDF
13C12 -1,2,3,4,7,8 -HxCDD
13C12 -1,2,3,4,7,8 -HxCDF
13C12-l,2,3,4,7,8,9-HpCDF
60
60
60
60
60
80
80
80
80
80
100
100
100
100
100
120
120
120
120
120
5
140
140
140
140
140
RECOVERY STANDARDS
13C12-1,2,3,4-TCDD
13C12 -1,2,3,7,8,9 -HxCDD
100
100
100
100
100
100
100
100
100
100
54
-------
TABLE 23-4. RECOMMENDED GC OPERATING CONDITIONS
Column Type
DB-5
DB-225
Length (m)
i . d . (mm)
Film Thickness (^m)
Carrier Gas
Carrier Gas Flow (mL/min)
60
0.25
0.25
Helium
1-2
30
0.25
0.25
Helium
1-2
Injection Mode
<-- splitless -->
Valve Time (min)
2.5
2.5
Initial Temperature (° C)
Initial Time (min)
Rate 1 (deg. C/min)
Temperature 2 (deg. C)
Rate 2 (deg. C/min)
Final Temperature (deg. C)
150
0.5
60
170
3
300
130
2.5
50
170
4
250
55
-------
TABLE 23-5. ELEMENTAL COMPOSITIONS AND EXACT MASSES OF THE IONS
MONITORED BY HIGH RESOLUTION MASS SPECTROMETRY FOR PCDD's AND PCDF's
DESCRIPTOR
NUMBER
2
*
3
ACCURATE
MASS
292.9825
303.9016
30,5.8987
315.9419
317.9389
319.8965
321.8936
327.8847
330.9792
331.9368
333.9339
339.8597
341.8567
351.9000
353.8970
355.8546
357.8516
367.8949
369.8919
375.8364
409.7974
373.8208
375.8178
383.8639
385.8610
389.8157
391.8127
392.9760
ION
TYPE
LOCK
M
M+2
M
M+2
M
M+2
M
QC
M
M+2
M+2
M+4
M+2
M+4
M+2
M+4
M+2
M+4
M+2
M+2
M+2
M+4
M
M+2
M+2
M+4
LOCK
ELEMENTAL COMPOSITION
C,Fu
C12H435C140
C12H435C13C1370
13C12H435C140
13C12H435C1337C10
C12H435C1402
C12H435C1337C102
C12H437C1402
C7F13
13C12H435C1402
13C12H43SC137C102
C12H335C1437C1O
C12H335C1337C120
13C12H335C1437C10
13C12H335C1337C120
C12H335C1337C102
C12H335C1337C1202
13C12H33SC1437C102
13C12H335C1337C1202
C12H435C1S37C10
C12H335C1637C10
C12H235C1537C1O
C12H235C1437C120
13C12H235C160
13C12H235C1537C10
C12H235C1537C102
C12H235C1437C1202
C9F15
ANALYTE
PFK
TCDF
TCDF
TCDF(S)
TCDF(S)
TCDD
TCDD
TCDD(S)
PFK
TCDD(S)
TCDD(S)
PeCDF
PeCDF
PeCDF (S)
PeCDF (S)
PeCDD
PeCDD
PeCDD (S)
PeCDD (S)
HxCDPE
HpCPDE
HxCDF
HxCDF
HxCDF (S)
HxCDF (S)
HxCDD
HxCDD
PFK
56
-------
401.8559
403.8529
445.7555
430.9729
M+2
M+4
M+4
QC
13C12H235C1537C102
13C12H235C1437C120
C12H235C1637C120
C9F17
HxCDD(S)
HxCDD(S)
OCDPE
PFK
TABLE 23-5.
(Continued)
DESCRIPTOR
NUMBER
ACCURATE
MASS
407.7818
409.7789
417.8253
389.8157
391.8127
392.9760
401.8559
403.8529
445.7555
430.9729
407.7818
409.7789
417.8253
419.8220
423.7766
425.7737
435.8169
437.8140
479.7165
430.9729
441.7428
443.7399
457.7377
459.7348
469.7779
ION
TYPE
M+2
M+4
M
M+2
M+4
LOCK
M+2
M+4
M+4
QC
M+2
M+4
M
M+2
M+2
M+4
M+2
M+4
M+4
LOCK
M+2
M+4
M+2
M+4
M+2
ELEMENTAL DESCRIPTION
C12H35C1637C1O
Ci2H35Cl537Cl2O
13C12H35C17O
C12H235C1537C102
C12H235C1437C1202
C9F15
13C12H235C1537C102
13C12H235C1437C120
C12H235C1637C120
C9F17
C12H35C1637C10
C12H35C1537C12O
13C12H35C170
13C12H35C1637C10
C12H35C1637C102
C12H35C1537C1202
13C12H35C1637C102
13C12H35C1537C1202
C12H35C1737C120
C9F17
C1235C1737C10
C1235C1637C120
C1235C1737C102
C123EC1637C1202
13C123SC1737C102
ANALYTE
HpCDF
HpCDF
HpCDF (S)
HxCDD
HxCDD
PFK
HxCDD (S)
HxCDD (S)
OCDPE
PFK
HpCDF
HpCDF
HpCDF (S)
HpCDF (S)
HpCDD
HpCDD
HpCDD (S)
HpCDD (S)
NCPDE
PFK
OCDF
OCDF
OCDD
OCDD
OCDD(S)
57
-------
471.7750
513.6775
442.9728
M+4
M+4
QC
13C1235C1637C1202
C1235C18"C1202
Cio^n
OCDD(S)
DCDPE
PFK
The following nuclidic masses were used:
H = 1.007825 0 = 15.994914 C = 12.000000 35C1 = 34.968853
13C = 13.003355 37C1 = 36.965903 F = 18.9984
S = Labeled Standard
QC = Ion selected for monitoring instrument stability during the
GC/MS analysis.
58
-------
TABLE 23-6. ACCEPTABLE RANGES FOR ION-ABUNDANCE RATIOS OF PCDD'S AND
PCDF'S
Number of
Chlorine
Atoms
4
5
6
6a
7b
7
8
Ion Type
M/M+2
M+2/M+4
M+2/M+4
M/M+2
M?M+2
M+2/M+4
M+2/M+4
Theoretical
Ratio
0.77
1.55
1.24
0.51
0.44
1.04
0.89
Control Limits
Lower
0.65
1.32
1.05
0.43
0.37
0.88
0.76
Upper
0.89
1.78
1.43
0.59
0.51
1.20
1.02
59
-------
TABLE 23-7. UNLABELED ANALYTES QUANTIFICATION RELATIONSHIPS
ANALYTE
2,3,7,8-TCDD
Other TCDD's
INTERNAL STANDARD USED
13C12-2,3,7,8-TCDD
13C12-2,3,7,8-TCDD
1,2,3,7,8-PeCDD
Other PeCDD's
13C12-l,2,3,7,8-PeCDD
13C12-l,2,3,7,8-PeCDD
1,2,3,4,7,8-HxCDD
1,2,3,6,7,8-HxCDD
1,2,3,7,8,9-HxCDD
Other HxCDD ' s
13C12-l,2,3,6,7,8-HxCDD
13C12-l,2,3,6,7,8-HxCDD
13C12- 1 ,2,3,6,7,8 -HxCDD
13C12-1 , 2,3,6,7, 8-HxCDD
1,2,3,4, 6,7, 8-HpCDD
1 Other HpCDD ' s
13C12 -1,2,3,4,6,7,8 -HpCDD
13C12 -1,2,3,4,6,7,8 -HpCDD
OCDD
13C12-OCDD
2,3,7,8-TCDF
Other TCDF ' s
13C12-2,3,7,8-TCDF
13C12-2,3,7,8-TCDF
1,2,3,7,8-PeCDF
2,3,4,7,8-PeCDF
Other PeCDF ' s
13C12-l,2,3,7,8-PeCDF
13C12-l,2,3,7,8-PeCDF
13C12-l,2,3,7,8-PeCDF
1,2,3,4,7,8-HxCDF
1,2,3,6,7,8-HxCDF
1,2,3,7,8, 9-HxCDF
2,3,4,6,7,8 -HxCDF
Other HxCDF 's
13C12 -1,2,3,6,7,8 -HxCDF
13C12- 1 ,2,3,6,7,8 -HxCDF
13C12-l,2,3,6,7,8-HxCDF
13C12-1,2,3,6,7,8-HXCDF
13C12 -1,2,3,6,7,8 -HxCDF
1,2,3,4,6,7,8-HpCDF
"C12-l,2,3,4,6,7,8-HpCDF |
60
-------
-s'L'9'fr'e'z'i-"o
ET
jaoo
8 ' Z. ' 9 ' fr ' £ ' Z ' I - "D
EI
- 6 '8'Z/fr'e'S'T
-------
TABLE 23-8. INTERNAL STANDARDS QUANTIFICATION RELATIONSHIPS
INTERNAL STANDARD
13C12-2,3,7,8-TCDD
13C12-l,2,3,7,8-PeCDD
13C12 - 1 , 2 , 3 , 6 , 7 , 8 - HxCDD
13C12 -1,2,3,4,6,7,8 -HpCDD
13C12-OCDD
13C12-2,3,7,8-TCDF
13C12-l,2,3,7,8-PeCDF
13C12-l,2,3,6,7,8-HxCDF
13C12- 1 ,2,3,4,6,7,8 -HpCDF
STANDARD USED DURING PERCENT
RECOVERY DETERMINATION
13C12-1,2,3,4-TCDD
13C12-1,2,3,4-TCDD
13C12-l,2,3,7,8,9-HxCDD
13C12 -1,2,3,7,8,9 -HxCDD
13C12 - 1 , 2 , 3 , 7 , 8 , 9 -HxCDD
13C12-1,2,3,4-TCDD
13C12-1,2,3,4-TCDD
13C12- 1 ,2,3,7,8,9 -HxCDD
13C12- 1 ,2,3,7,8,9 -HxCDD
TABLE 23-9. SURROGATE STANDARDS QUANTIFICATION RELATIONSHIPS
SURROGATE STANDARD
37Cl4-2,3,7,8-TCDD
13C12-2,3,4,7,8-PeCDF
13C12-l,2,3,4,7,8-HxCDD
13C12 -1,2,3,4,7,8 -HxCDF
13C12-l,2,3,4,7,8,9-HpCDF
STANDARD USED DURING PERCENT
RECOVERY DETERMINATION
13C12-2,3,7,8-TCDD
13C12- 1 ,2,3,7,8- PeCDF
13C12- 1 ,2,3,6,7,8 -HxCDD
13C12 -1,2,3,6,7,8 -HxCDF
13C12-l,2,3,4,6,7,8-HpCDF
62
-------
TABLE 23-10. MINIMUM REQUIREMENTS FOR INITIAL AND DAILY CALIBRATION
RESPONSE FACTORS
COMPOUND
RELATIVE RESPONSE FACTORS
INITIAL
CALIBRATION
(RSD)
DAILY
CALIBRATION
(% DIFFERENCE)
UNLABELED ANALYTES
2,3,7,8-TCDD
2,3,7, 8-TCDF
1,2,3,7,8-PeCDD
1,2,3,7,8-PeCDF
1,2,4,5,7,8-HxCDD
1,2,3,6,7,8-HxCDD
1,2,3,7,8,9-HxCDD
1,2,3,4,7,8-HxCDF
1,2,3,6,7,8-HxCDF
1,2,3,7,8,9-HxCDF
2,3,4,6,7,8-HxCDF
1,2,3,4,6,7,8-HpCDD
1,2,3,4,6, 7,8 -HpCDF
OCDD
OCDF
25
25
25
25
25
25
25
25
25
25
25
25
25
25
30
25
25
25
25
25
25
25
25
25
25
25
25
25
25
30
SURROGATE STANDARDS
37Cl4-2,3,7,8-TCDD
13C12-2,3,4,7,8-PeCDF
13C12 - 1 , 2 , 3 , 4 , 7 , 8 -HxCDD
13C12- 1 ,2,3,4,7,8 -HxCDF
13C12-l,2,3,4,7,8,9-HpCDF
25
25
63
-------
»T
H-
IQ
(D
H
Thermocouple
"8" Type Pilot
Filler Holder
Thermocouple
Probe
Thermocouple Thermocouple
/ Cheek Valve
Sleek Wall /
Pilot
a\
(300 grama)
lee Beth
Implngtr
Thermocouplee
Orifice
Manometer .«*• . .
ReclrculatlbnPump WA(ar Knockout 100ml HPLC Water
Vacuum Line
Air-Tight
Pump
Figure 5-1. CDD/CDF Sampling Train Configuration
-------
h:
H-
Condenaar
Flue Gas Flow •
Sorbant Trap
CD
to
•20/18
37cm-
8 mm QlaM Cooling Coll
To Suit-
•••••••••• y^^^^*"1"""!
•••••••••• .X7
»••••*••••§ L<< y
_ - * - ^ ^
•20/18
Wafer Jacket Cooling Colt
QlaM Wool Plug Watar Jacket XAD • 2
(76 Grams)
Gtaaa Slntarad Disk
FIGURE 2. CONDENSER AND SORBENT TRAP FOR COLLECTION OF GASEOUS PCDDt AND
PCDFa
-------
Appendix G.6
EPA Method 25A
-------
EMISSION MEASUREMENT TECHNICAL INFORMATION CENTER
NSP8 TKST KBTBOD
METHOD 25A-DKTKRIiI naTIOH OF TOTAL GASEOUS ORGANIC
CONCENTRATION USING A FLAME IONIZATION ANALYZER
1. Applicability and Principle
1.1 Applicability. This method applies to the measurement of total gaseous
organic concentration of vapors consisting primarily of alkanes, alkenes, and/or
arenes (aromatic hydrocarbons). The concentration is expressed in terms of
propane (or other appropriate organic calibration gas) or in terms of carbon.
1.2 Principle. A gas sample is extracted from the source through a heated
sample line, if necessary, and glass fiber filter to a flame ionization analyzer
(FIA) . Results are reported as volume concentration equivalents of the
calibration gas or as carbon equivalents.
•
2. Definitions
2.1 Measurement Systems. The total equipment required for the determination
of the gas concentration. The system consists of the following major subsystems:
2.1.1 Sample Interface. That portion of the system that is used for one or more
of the following: sample acquisition, sample transportation, sample
conditioning, or protection of the analyzer from the effects of the stack
effluent.
2.1.2 Organic Analyzer. That portion of the system that senses organic
concentration and generates an output proportional to the gas concentration.
2.2 Span Value. The upper limit of a gas concentration measurement range that
is specified for affected source categories in the applicable part of the
regulations. The span value is established in the applicable regulation and is
usually 1.5 to 2.5 times the applicable emission limit. If no span value is
provided, use a span value equivalent to 1.5 to 2.5 times the expected
concentration. For convenience, the span value should correspond to 100 percent
of the recorder scale.
2.3 Calibration Gas. A known concentration of a gas in an appropriate diluent
gas.
2.4 Zero Drift. The difference in the measurement system response to a zero
level calibration gas before and after a stated period of operation during which
no unscheduled maintenance, repair, or adjustment took place.
Prepared by Emission Measurement Branch EMTIC TM-25A
Technical Support Division, OAQPS, EPA June 23, 1993
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EMTIC TM-25A EMTIC NSPS TEST METHOD Page 2
2.5 Calibration drift. The difference in the measurement system response to
a midlevel calibration gas before and after a stated period of operation during
which no unscheduled maintenance, repair or adjustment took place.
2.6 Response Time. The time interval from a step change in pollutant
concentration at the inlet to the emission measurement system to the time at
which 95 percent of the corresponding final value is reached as displayed on the
recorder.
2.7 Calibration Error. The difference between the gas concentration indicated
by the measurement system and the known concentration of the calibration gas.
3. Apparatus.
A schematic of an acceptable measurement system is shown in Figure 25A-1.
The essential components of the measurement system are described below:
3.1* Organic Concentration Analyzer. A flame ionization analyzer (FIA) capable
of meeting or exceeding the specifications in this method.
3.2 Sample Probe. Stainless steel, or equivalent, three-hole rake type.
Sample holes shall be 4 mm in diameter or smaller and located at 16.7, 50, and
83.3 percent of the equivalent stack diameter. Alternatively, a single opening
probe may be used so that a gas sample is collected from the centrally located
10 percent area of the stack cross-sect ion.
3.3 Sample Line. Stainless steel or Teflon * tubing to transport the sample
gas to the analyzer. The sample line should be heated, if necessary, to prevent
condensation in the line.
3.4 Calibration Valve Assembly. A three way valve assembly to direct the zero
and calibration gases to the analyzers is recommended. Other methods, such as
quick-connect lines, to route calibration gas to the analyzers are applicable.
3.5 Particulate rilter. An in-stack or an out-of-stack glass fiber filter is
recommended if exhaust gas particulate loading is significant. An out-of-stack
filter should be heated to prevent any condensation.
* Mention of trade names or specific products does not constitute
endorsement by the Environmental Protection Agency.
3.6 Recorder. A strip-chart recorder, analog computer, or digital recorder for
recording measurement data. The minimum data recording requirement is one
measurement value per minute. Note: This method is often applied in highly
explosive areas. Caution and care should be exercised in choice of equipment and
installation.
4. Calibration and Other Oases.
Oases used for calibrations, fuel, and combustion air (if required) are
-------
EMTIC TM-25A EMTIC NSPS TEST METHOD Page 3
contained in compressed gas cylinders. Preparation of calibration gases shall
be done according to the procedure in Protocol No. 1, listed in Citation 2 of
Bibliography. Additionally, the manufacturer of the cylinder should provide a
recommended shelf life for each calibration gas cylinder over which the
concentration does not change more than ±2 percent from the certified value. For
calibration gas values not generally available (i.e., organics between 1 and 10
percent by volume), alternative methods for preparing calibration gas mixtures,
such as dilution systems, may be used with prior approval of the Administrator.
Calibration gases usually consist of propane in air or nitrogen and are
determined in terms of the span value. Organic compounds other than propane can
be used following the above guidelines and making the appropriate corrections for
response factor.
4.1 Fuel. A 40 percent H2/60 percent 1% gas mixture is recommended to avoid
an oxygen synergism effect that reportedly occurs when oxygen concentration
varies significantly from a mean value.
4.2 Zero Gas. High purity air with less than 0.1 parts per million by volume
(ppmv) of organic material (propane or carbon equivalent) or less than 0.1
percent of the span value, whichever is greater.
4.3 Low-level Calibration Gas. An organic calibration gas with a concentration
equivalent to 25 to 35 percent of the applicable span value.
4.4 Mid-level Calibration Gas. An organic calibration gas with a concentration
equivalent to 45 to 55 percent of the applicable span value.
4.5 High-level Calibration Gas. An organic calibration gas with a
concentration equivalent to 80 to 90 percent of the applicable span value.
5. Measurement System Performance Specifications
5.1 Zero Drift. Less than ±3 percent of the span value.
5.2 Calibration Drift. Less than ±3 percent of span value.
5.3 Calibration Error. Less than ±5 percent of the calibration gas value.
6. Pretest Preparations
6.1 Selection of Sampling Site. The location of the sampling site is generally
specified by the applicable regulation or purpose of the test; i.e., exhaust
stack, inlet line, etc. The sample port shall be located at least 1.5 meters or
2 equivalent diameters upstream of the gas discharge to the atmosphere.
6.2 Location of Sample Probe. Install the sample probe so that the probe is
centrally located in the stack, pipe, or duct and is sealed tightly at the stack
port connection.
-------
EHTXC TM-25A EMTIC NSPS TEST METHOD Page 4
6.3 Measurement System Preparation. Prior to the emission test, assemble the
measurement system following the manufacturer's written instructions in preparing
the sample interface and the organic analyzer. Make the system operable.
FIA equipment can be calibrated for almost any range of total organica
concentrations. For high concentrations of organics (>1.0 percent by volume as
propane) modifications to most commonly available analyzers are necessary. One
accepted method of equipment modification is to decrease the size of the sample
to the analyzer through the use of a smaller diameter sample capillary. Direct
and continuous measurement of organic concentration is a necessary consideration
when determining any modification design.
6.4 Calibration Krror Test. Immediately prior to the test series, (within 2
hours of the start of the test) introduce zero gas and high-level calibration gas
at the calibration valve assembly. Adjust the analyzer output to the appropriate
levels, if necessary. Calculate the predicted response for the low-level and
mid-level gases based on a linear response line between the zero and high-level
responses. Then introduce low-level and mid-level calibration gases successively
to the measurement system. Record the analyzer responses for low-level and mid-
level calibration gases and determine the differences between the measurement
system responses and the predicted responses. These differences must be less
than S percent of the respective calibration gas value. If not, the measurement
system is not acceptable and must be replaced or repaired prior to testing. No
adjustments to the measurement system shall be conducted after the calibration
and before the drift check (Section 7.3). If adjustments are necessary before
the completion of the test series, perform the drift checks prior to the required
adjustments and repeat the calibration following the adjustments. If multiple
electronic ranges are to be used, each additional range must be checked with a
mid-level calibration gas to verify the multiplication factor.
6.5 Response Time Test. Introduce Zero gas into the measurement system at the
calibration valve assembly. When the system output has stabilized, switch
quickly to the high-level calibration gas. Record the time from the
concentration change to the measurement system response equivalent to 95 percent
of the step change. Repeat the test three times and average the results.
7. Emission Measurement Test Procedure
7.1 Organic Measurement. Begin sampling at the start of the test period,
recording time and any required process information as appropriate. In
particular, note on the recording chart periods of process interruption or cyclic
operation.
7.2 Drift Determination. Immediately following the completion of the test
period and hourly during the test period, reintroduce the zero and mid-level
calibration gases, one at a time, to the measurement system at the calibration
valve assembly. (Make no adjustments to the measurement system until after both
the zero and calibration drift checks are made.) Record the analyzer response.
If the drift values exceed the specified limits, invalidate the test results
preceding the check and repeat the test following corrections to the measurement
-------
EMTIC TM-25A EMTIC NSPS TEST METHOD Page 5
system. Alternatively, recalibrate the test measurement system as in Section 6.4
and report the results using both sets of calibration data (i.e., data determined
prior to the test period and data determined following the test period) .
8. Organic Concentration calculations
Determine the average organic concentration in terms of ppmv as propane or
other calibration gas. The average shall be determined by the integration of the
output recording over the period specified in the applicable regulation. If
results are required in terms of ppmv as carbon, adjust measured concentrations
using Equation 25A-1.
Eq. 25A-1
Where:
Ce • Organic concentration as carbon, ppmv.
CM.,- Organic concentration as measured, ppmv.
K • Carbon equivalent correction factor.
K - 2 for ethane.
K - 3 for propane.
K - 4 for butane.
K • Appropriate response factor for other organic calibration
gases.
9. Bibliography
1. Measurement of Volatile Organic Compounds-Guideline Series. U.S.
Environmental Protection Agency. Research Triangle Park, NC.
Publication No. EPA-450/2-78-041. June 1978. p. 46-54.
2. Traceability Protocol for Establishing True Concentrations of Gases
Used for Calibration and Audits of Continuous Source Emission
Monitors (Protocol No. 1) . U.S. Environmental Protection Agency,
Environmental Monitoring and Support Laboratory. Research Triangle
Park, NC. June 1978.
3. Gasoline Vapor Emission Laboratory Evaluation-Part 2. U.S.
Environmental Protection Agency, Office of Air Quality Planning and
Standards. Research Triangle Park, NC. EMB Report No. 75-GAS-6.
August 1975.
-------
EMTIC TM-25A
EMTIC NSPS TEST METHOD
Page 6
PR**
Organic
Analyzer
Pump
Stack
Figure 25A-1. Organic Concentration Measurement System.
-------
Appendix G.7
EPA Method 26A
-------
Method 26A - Determination of Hydrogen Halide and Halogen Emissions
from Stationary Sources - Isokinetic Method
1. APPLICABILITY, PRINCIPLE, INTERFERENCES, PRECISION, BIAS, AND
STABILITY
1.1 Applicability. This method is applicable for
determining emissions of hydrogen halides (HX) [hydrogen chloride
(HCl), hydrogen bromide (HBr), and hydrogen fluoride (HF)] and
halogens (X2) [chlorine (C12) and bromine (Br2)] from stationary
sources. This method collects the emission sample isokinetically
and.is therefore particularly suited for sampling at sources,
such as those controlled by wet scrubbers, emitting acid
particulate matter (e.g., hydrogen halides dissolved in water
droplets). [Note: Mention of trade names or specific products
does not constitute endorsement by the Environmental Protection
Agency.]
1.2 Principle. Gaseous and particulate pollutants are
withdrawn isokinetically from the source and collected in an
optional cyclone, on a filter, and in absorbing solutions. The
cyclone collects any liquid droplets and is not necessary if the
source emissions do not contain them; however, it is preferable
to include the cyclone in the sampling train to protect the
filter from any moisture present. The filter collects other
particulate matter including halide salts. Acidic and alkaline
-------
absorbing solutions collect the gaseous hydrogen halides and
halogens, respectively. Following sampling of emissions
containing liquid droplets, any halides/halogens dissolved in the
liquid in the cyclone and on the filter are vaporized to gas and
collected in the impingers by pulling conditioned ambient air
through the sampling train. The hydrogen halides are solubilized
in the acidic solution and form chloride (Cl~) , bromide (Br~) ,
and fluoride (F~) ions. The halogens have a very low solubility
in the acidic solution and pass through to the alkaline solution
where they are hydrolyzed to form a proton (H+) , the halide ion,
and the hypohalous acid (HC1O or HBrO). Sodium thiosulfate is
added to the alkaline solution to assure reaction with the
hypohalous acid to form a second halide ion such that 2 halide
ions are formed for each molecule of halogen gas. The halide ions
in the separate solutions are measured by ion chromatography
(1C). If desired, the particulate matter recovered from the
filter and the probe is analyzed following the procedures in
Method 5. [Note.- If the tester intends to use this sampling
arrangement to sample concurrently for particulate matter, the
alternative TeflonR probe liner, cyclone, and filter holder
should not be used. The TeflonR filter support must be used.
The tester must also meet the probe and filter temperature
requirements of both sampling trains.]
-------
1.3 Interferences. Volatile materials, such as chlorine
dioxide (C102) and ammonium chloride (NH4C1), which produce
halide ions upon dissolution during sampling are potential
interferents. Interferents for the halide measurements are the
halogen gases which disproportionate to a hydrogen halide and an
hypohalous acid upon dissolution in water. The use of acidic
rather than neutral or basic solutions for collection of the
hydrogen halides greatly reduces the dissolution of any halogens
passing through this solution. The simultaneous presence of both
HBr and C12 may cause a positive bias in the HC1 result with a
corresponding negative bias in the C12 result as well as
affecting the HBr/Br2 split. High concentrations of nitrogen
oxides (NOX) may produce sufficient nitrate (NO3~) to interfere
with measurements of very low Br~ levels.
1.4 Precision and Bias. The method has a possible
measurable negative bias below 20 ppm HC1 perhaps due to reaction
with small amounts of moisture in the probe and filter. Similar
bias for the other hydrogen halides is possible.
1.5 Sample Stability. The collected Cl~ samples can be
stored for up to 4 weeks for analysis for HC1 and C12.
1.6 Detection Limit. The in-stack detection limit for HCl
is approximately 0.02 /ig per liter of stack gas; the analytical
detection limit for HCl is 0.1 /xg/ml. Detection limits for the
-------
other analyses should be similar.
2. APPARATUS
2.1 Sampling. The sampling train is shown in Figure 26A-1;
the apparatus is similar to the Method 5 train where noted as
follows:
Holed
Teflon or Quartz
Filter
Dry Qu Vacuum
Meter Pump
Figure 26A-1. Sampling Train
-------
2.1.1 Probe Nozzle. Borosilicate or-quartz glass;
constructed and calibrated according to Method 5, Sections 2.1.1
and 5.1, and coupled to the probe liner using a TeflonR union; a
stainless steel nut is recommended for this union. When the
stack temperature exceeds 210°C (410°F) , a one-piece glass
nozzle/liner assembly must be used.
2.1.2 Probe Liner. Same as Method 5, Section 2.1.2, except
metal liners shall not be used. Water-cooling of the stainless
steel sheath is recommended at temperatures exceeding 500°C.
TeflonR may be used in limited applications where the minimum
stack temperature exceeds 120 °C (250 °F) but never exceeds the
temperature where TeflonR is estimated to become unstable
(approximately 210 °C) .
2.1.3 Pitot Tube, Differential Pressure Gauge, Filter
Heating System, Metering System, Barometer, Gas Density
Determination Equipment. Same as Method 5, Sections 2.1.3,
2.1.4, 2.1.6, 2.1.8, 2.1.9, and 2.1.10.
2.1.4 Cyclone (Optional). Glass or TeflonR . Use of the
cyclone is required only when the sample gas stream is saturated
with moisture; however, the cyclone is recommended to protect 'the
filter from any moisture droplets present.
2.1.5 Filter Holder. Borosilicate or quartz glass, or
-------
TeflonR filter holder, with a TeflonR filter support and a
sealing gasket. The sealing gasket shall be constructed of
TeflonR or equivalent materials. The holder design shall provide
a positive seal against leakage at any point along the filter
circumference. The holder shall be attached immediately to the
outlet of the cyclone.
2.1.6 Impinger Train. The following system shall be used
to determine the stack gas moisture content and to collect the
hydrogen halides and halogens: five or six impingers connected
in series with leak-free ground glass fittings or any similar
leak-free noncontaminating fittings. The first impinger shown in
Figure 26A-1 (knockout or condensate impinger) is optional and is
recommended as a water knockout trap for use under high moisture
conditions. If used, this impinger should be constructed as
described below for the alkaline impingers, but with a shortened
stem, and should contain 50 ml of 0.1 N H2SO4. The following two
impingers (acid impingers which each contain 100 ml of 0.1 N
H2SO4) shall be of the Greenburg-Smith design with the standard
tip (Method 5, Section 2.1.7). The next two impingers (alkaline
impingers which each contain 100 ml of 0.1 N NaOH) and the last
impinger (containing silica gel) shall be of the modified
Greenburg-Smith design (Method 5, Section 2.1.7). The
condensate, acid, and alkaline impingers shall contain known
-------
quantities of the appropriate absorbing reagents. The last
impinger shall contain a known weight of silica gel or equivalent
desiccant. TeflonR impingers are an acceptable alternative.
2.1.7 Ambient Air Conditioning Tube (Optional). Tube
tightly packed with approximately 150 g of fresh 8 to 20 mesh
sodium hydroxide-coated silica, or equivalent, (Ascarite IIR has
been found suitable) to dry and remove acid gases from the
ambient air used to remove moisture from the filter and cyclone,
when the cyclone is used. The inlet and outlet ends of the tube
should be packed with at least 1-cm thickness of glass wool or
filter material suitable to prevent escape of fines. Fit one end
with flexible tubing, etc. to allow connection to probe nozzle
following the test run.
2.2 Sample Recovery. The following items are needed:
2.2.1 Probe-Liner and Probe-Nozzle Brushes, Wash Bottles,
Glass Sample Storage Containers, Petri Dishes, Graduated Cylinder
or Balance, and Rubber Policeman. Same as Method 5, Sections
2.2.1, 2.2.2, 2.2.3, 2.2.4, 2.2.5, and 2.2.7.
2.2.2 Plastic Storage Containers. Screw-cap polypropylene
or polyethylene containers to store silica gel. High-density
polyethylene bottles with Teflon screw cap liners to store
impinger reagents, 1-liter.
2.2.3 Funnels. Glass or high-density polyethylene, to aid
-------
in sample recovery.
2.3 Analysis. For analysis, the following equipment is
needed:
2.3.1 Volumetric Flasks. Class A, various sizes.
2.3.2 Volumetric Pipettes. Class A, assortment, to dilute
samples to calibration range of the ion chromatograph (1C) .
2.3.3 Ion Chromatograph. Suppressed or nonsuppressed, with
a conductivity detector and electronic integrator operating in
the peak area mode. Other detectors, a strip chart recorder, and
peak heights may be used.
3. REAGENTS
Unless otherwise indicated, all reagents must conform to the
specifications of the Committee on Analytical Reagents of the
American Chemical Society (ACS reagent grade). When such
specifications are not available, the best available grade shall
be used.
3.1 Sampling.
3.1.1 Water. Deionized, distilled water that conforms to
American Society of Testing and Materials (ASTM) Specification D
1193-77, Type 3.
3.1.2 Acidic Absorbing Solution, 0.1 N Sulfuric Acid
(H2S04) . To prepare 1 L, slowly add 2.80 ml of concentrated H2SO,
to about 900 ml of water while stirring, and adjust the final
-------
volume to 1 L using additional water. Shake well to mix the
solution.
3.1.3 Alkaline Absorbing Solution, 0.1 N Sodium Hydroxide
(NaOH). To prepare 1 L, dissolve 4.00 g of solid NaOH in about
900 ml of water and adjust the final volume to 1 L using
additional water. Shake well to mix the solution.
3.1.4 Filter. TeflonR mat (e.g., PallflexR TX40HI45)
filter. When the stack gas temperature exceeds 210 °C (410 °F) a
quartz fiber filter may be used.
*
3.1.5 Silica Gel, Crushed Ice, and Stopcock Grease. Same
as Method 5, Sections 3.1.2, 3.1.4, and 3.1.5, respectively.
3.1.6 Sodium Thiosulfate, (Na2S2033-5 H20) .
3.2 Sample Recovery.
3.2.1 Water. Same as Section 3.1.1.
3.2.2 Acetone. Same as Method 5, Section 3.2.
3.3 Sample Analysis.
3.3.1 Water. Same as Section 3.1.1.
3.3.2 Reagent Blanks. A separate blank solution of each
absorbing reagent should be prepared for analysis with the field
samples. Dilute 200 ml of each absorbing solution (250 ml of the
acidic absorbing solution, if a condensate impinger is used) to
the same final volume as the field samples using the blank sample
of rinse water. If a particulate determination is conducted,
-------
collect a blank sample of acetone.
3.3.3 Halide Salt Stock Standard Solutions. Prepare
concentrated stock solutions from reagent grade sodium chloride
(NaCl), sodium bromide (NaBr), and sodium fluoride (NaF). Each
must be dried at 110°C for 2 or more hours and then cooled to .
room temperature in a desiccator immediately before weighing.
Accurately weigh 1.6 to 1.7 g of the dried NaCl to within 0.1 mg,
dissolve in water, and dilute to 1 liter. Calculate the exact
Cl" concentration using Equation 26A-1.
/xg Cl'/ml = g of NaCl x 103 x 35.453/58.44 Eq. 26A-1
In a similar manner, accurately weigh and solubilize 1.2 to 1.3 g
of dried NaBr and 2.2 to 2.3 g of NaF to make 1-liter solutions.
Use Equations 26A-2 and 26A-3 to calculate the Br~ and F~
concentrations.
(j.g Br-/ml = g of NaBr x 103 x 79.904/102.90 Eq. 26A-2
/xg F-/ml = g of NaF x 103 x 18.998/41.99 Eq. 26A-3
Alternately, solutions containing a nominal certified
concentration of 1000 mg/L NaCl are commercially available as
convenient stock solutions from which standards can be made by
appropriate volumetric dilution. Refrigerate the stock standard
solutions and store no longer than 1 month.
3.3.4 Chromatographic Eluent. Same as Method 26, Section
3.2.4.
-------
4. PROCEDURE
Because of the complexity-,of this method, testers and
analysts should be trained and experienced with the procedures to
ensure reliable results.
4.1 Sampling.
4.1.1 Pretest Preparation. Follow the general procedure
given in Method 5, Section 4.1.1, except the filter need only be
desiccated and weighed if a particulate determination will be
conducted.
4.1.2 Preliminary Determinations. Same as Method 5,
Section 4.1.2.
4.1.3 Preparation of Sampling Train. Follow the general
procedure given in Method 5, Section 4.1.3, except for the
following variations:
Add 50 ml of 0.1 N H2S04 to the condensate impinger, if
used. Place 100 ml of 0.1 N H2SO4 in each of the next two
impingers. Place 100 ml of 0.1 N NaOH in each of the following
two impingers. Finally, transfer approximately 200-300 g of
preweighed silica gel from its container to the last impinger.
Set up the train as in Figure 26A-1. When used, the optional
cyclone is inserted between the probe liner and filter holder and
located in the heated filter box.
4.1.4 Leak-Check Procedures. Follow the leak-check
-------
procedures given in Method 5, Sections 4.4.1 (Pretest Leak-
Check), 4.1.4.2 (Leak-Checks During the Sample Run), and 4.1.4.3
(Post-Test Leak-Check).
4.1.5 Train Operation. Follow the general procedure given
in Method 5, Section 4.1.5. Maintain a temperature around the
filter and (cyclone, if used) of greater than 120 °C (248 °F) .
For each run, record the data required on a data sheet such as
the one shown in Method 5, Figure 5-2. If the condensate
impinger becomes too full, it may be emptied, recharged with
50 ml of 0.1 N H2S04, and replaced during the sample run. The
condensate emptied must be saved and included in the measurement
of the volume of moisture collected and included in the sample
for analysis. The additional 50 ml of absorbing reagent must
also be considered in calculating the moisture. After the
impinger is reinstalled in the train, conduct a leak-check as
described in Method 5, Section 4.1.4.2.
4.1.6 Post-Test Moisture Removal (Optional). When the
optional cyclone is included in the sampling train or when
moisture is visible on the filter at the end of a sample run even
in the absence of a cyclone, perform the following procedure.
Upon completion of the test run, connect the ambient air
conditioning tube at the probe inlet and operate the train with
the filter heating system at least 120 °C (248 °F) at a low flow
-------
rate (e.g., AH = 1 in. H2O) to vaporize any liquid and hydrogen
halides in the cyclone or on the filter and .pull them through the
train into the impingers. After 30 minutes, turn off the flow,
remove the conditioning tube, and examine the cyclone and filter
for any visible moisture. If moisture is visible, repeat this
step for 15 minutes and observe again. Keep repeating until the
cyclone is dry. [Note: It is critical that this is repeated
until the cyclone is completely dry.]
4.2 Sample Recovery. Allow the probe to cool. When the
probe can be handled safely, wipe off all the external surfaces
of the tip of the probe nozzle and place a cap loosely over the
tip. Do not cap the probe tip tightly while the sampling train
is cooling down because this will create a vacuum in the filter
holder, drawing water from the impingers into the holder. Before
moving the sampling train to the cleanup site, remove the probe,
wipe off any silicone grease, and cap the open outlet of the
impinger train, being careful not to lose any condensate that
might be present. Wipe off any silicone grease and cap the
filter or cyclone inlet. Remove the umbilical cord from the last
impinger and cap the impinger. If a flexible line is used
between the first impinger and the filter holder, disconnect it
at the filter holder and let any condensed water drain into the
first impinger. Wipe off any silicone grease and cap the filter
-------
holder outlet and the impinger inlet. Ground glass stoppers,
plastic caps, serum caps, TeflonR tape, ParafilmR, or aluminum
foil may be used to close these openings. Transfer the probe and
filter/impinger assembly to the cleanup area. This area should
be clean and protected from the weather to minimize sample
contamination or loss. Inspect the train prior to and during
disassembly and note any abnormal conditions. Treat samples as
follows:
4.2.1 Container No. 1 (Optional; Filter Catch for
Particulate Determination). Same as Method 5, Section 4.2,
Container No. 1.
4.2.2 Container No. 2 (Optional; Front-Half Rinse for
Particulate Determination). Same as Method 5, Section 4.2,
Container No. 2.
4.2.3 Container No. 3 (Knockout and Acid Impinger Catch for
Moisture and Hydrogen Halide Determination). Disconnect the
impingers. Measure the liquid in the acid and knockout impingers
to ±1 ml by using a graduated cylinder or by weighing it to ±0.5
g by using a balance. Record the volume or weight of liquid
present. This information is required to calculate the moisture
content of the effluent gas. Quantitatively transfer this liquid
to a leak-free sample storage container. Rinse these impingers
and connecting glassware including the back portion of the filter
-------
holder (and flexible tubing, if used) with water and add these
rinses to the storage container. Seal the container, shake to
mix, and label. The fluid level should be marked so that if any
sample is lost during transport, a correction proportional to the
lost volume can be applied. Retain rinse water and acidic
absorbing solution blanks and analyze with the samples.
4.2.4 Container No. 4 (Alkaline Impinger Catch for Halogen
and Moisture Determination). Measure and record the liquid in
the alkaline impingers as described in Section 4.2.3.
Quantitatively transfer this liquid to a leak-free sample storage
container. Rinse these two impingers and connecting glassware
with water and add these rinses to the container. Add 25 mg of
sodium thiosulfate per ppm halogen-dscm of stack gas sampled.
[Note: This amount of sodium thiosulfate includes a safety
factor of approximately 5 to assure complete reaction with the
hypohalous acid to form a second Cl" ion in the alkaline
solution.] Seal the container, shake to mix, and label; mark
the fluid level. Retain alkaline absorbing solution blank and
analyze with the samples.
4.2.5 Container No. 5 (Silica Gel for Moisture
Determination). Same as Method 5, Section 4.2, Container No. 3.
4.2.6 Container Nos. 6 through 9 (Reagent Blanks). Save
portions of the absorbing reagents (0.1 N H2SO4 and 0.1 N NaOH)
-------
equivalent to the amount used in the sampling train; dilute to
the approximate volume of the corresponding samples using rinse
water directly from the wash bottle being used. Add the same
ratio of sodium thiosulfate solution used in container No. 4 to
the 0.1 N NaOH absorbing reagent blank. Also, save a portion of
the rinse water alone and a portion of the acetone equivalent to
the amount used to rinse the front half of the sampling train.
Place each in a separate, prelabeled sample container.
4.2.7 Prior to shipment, recheck all sample containers to
ensure that the caps are well-secured. Seal the lids of all
containers around the circumference with TeflonR tape. Ship all
liquid samples upright and all particulate filters with the
particulate catch facing upward.
4.3 Sample Preparation and Analysis. Note the liquid
levels in the sample containers and confirm on the analysis sheet
whether or not leakage occurred during transport. If a
noticeable leakage has occurred, either void the sample or use
methods, subject to the approval of the Administrator, to correct
the final results.
4.3.1 Container Nos. 1 and 2 and Acetone Blank (Optional;
Particulate Determination). Same as Method 5, Section 4.3.
4.3.2 Container No. 5. Same as Method 5, Section 4.3 for
silica gel.
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4.3.3 Container Nos. 3 and 4 and Absorbing Solution and
Water Blanks. Quantitatively.transfer each sample to a
volumetric flask or graduated cylinder and dilute with water to a
final volume within 50 ml of the largest sample.
4.3.3.1 The 1C conditions will depend upon analytical
column type and whether suppressed or nonsuppressed 1C is used.
Prior to calibration and sample analysis, establish a stable
baseline. Next, inject a sample of water, and determine if any
Cl',% Br~, or F~ appears in the chromatogram. If any of these ions
are present, repeat the load/injection procedure until they are
no longer present. Analysis of the acid and alkaline absorbing
solution samples requires separate standard calibration curves;
prepare each according to Section 5.2. Ensure adequate baseline
separation of the analyses.
4.3.3.2 Between injections of the appropriate series of
calibration standards, inject in duplicate the reagent blanks and
the field samples. Measure the areas or heights of the Cl", Br",
and F~ peaks. Use the average response to determine the
concentrations of the field samples and reagent blanks using the
linear calibration curve. If the values from duplicate
injections are not within 5 percent of their mean, the duplicate
injection shall be repeated and all four values used to determine
the average response. Dilute any sample and the blank with equal
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volumes of water if the concentration exceeds that of the highest
standard.
4.4 Audit Sample Analysis. Audit samples must be analyzed
subject to availability.
5. CALIBRATION
Maintain a laboratory log of all calibrations.
5.1 Probe Nozzle, Pitot Tube, Dry Gas Metering System,
Probe Heater, Temperature Gauges, Leak-Check of Metering System,
and Barometer. Same as Method 5, Sections 5.1, 5.2, 5.3, 5.4,
•
5.5, 5.6, and 5.7, respectively.
5.2 Ion Chromatograph. To prepare the calibration
standards, dilute given amounts (1.0 ml or greater) of the stock
standard solutions to convenient volumes, using 0.1 N H2SO4 or
0.1 N NaOH, as appropriate. Prepare at least four calibration
standards for each absorbing reagent containing the three stock
solutions such that they are within the linear range of the field
samples. Using one of the standards in each series, ensure
adequate baseline separation for the peaks of interest. Inject
the appropriate series of calibration standards, starting with
the lowest concentration standard first both before and after
injection of the quality control check sample, reagent blanks,
and field samples. This allows compensation for any instrument
drift occurring during sample analysis. Determine the peak
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areas, or height, of the standards and plot individual values
versus halide ion concentrations in pig/ml. Draw a smooth curve
through the points. Use linear regression to calculate a formula
describing the resulting linear curve.
6. QUALITY CONTROL
Same as Method 5, Section 4.4.
7. QUALITY ASSURANCE
7.1 Applicability. When the method is used to demonstrate
compliance with a regulation, a set of two audit samples shall be
analyzed.
7.2 Audit Procedure. The currently available audit samples
are chloride solutions. Concurrently analyze the two audit
samples and a set of compliance samples in the same manner to
evaluate the technique of the analyst and the standards
preparation. The same analyst, analytical reagents, and
analytical system shall be used both for compliance samples and
the Environmental Protection Agency (EPA) audit samples.
7.3 Audit Sample Availability. Audit samples will be
supplied only to enforcement agencies for compliance tests.
Audit samples may be obtained by writing the Source Test Audit
Coordinator (MD-77B), Quality Assurance Division, Atmospheric
Research and Exposure Assessment Laboratory, U.S. Environmental
Protection Laboratory, Research Triangle Park, NC 27711 or by
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calling the Source Test Audit Coordinator (STAC) at
(919) 541-7834. The request for the audit samples should be made
at least 30 days prior to the scheduled compliance sample
analysis.
7.4 Audit Results. Calculate the concentrations in mg/dscm
using the specified sample volume in the audit instructions.
Include the results of both audit samples, their identification
numbers, and the analyst's name with the results of the
compliance determination samples in appropriate reports to the
*
EPA regional office or the appropriate enforcement agency.
(NOTE: Acceptability of results may be obtained immediately by
reporting the audit results in mg/dscm and compliance results in
total fj.g HCl/sample to the responsible enforcement agency.) The
concentrations of the audit samples obtained by the analyst shall
agree within 10 percent of the actual concentrations. If the
10 percent specification is not met, reanalyze the compliance
samples and audit samples, and include initial and reanalysis
values in the test report. Failure to meet the 10 percent
specification may require retests until the audit problems are
resolved.
8. CALCULATIONS
Retain at least one extra decimal figure beyond those
contained in the available data in intermediate calculations, and
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round off only the final answer appropriately.
8.1 Nomenclature. Same, as Method 5,. Section 6.1. In
addition:
1 Bx- = Mass concentration of applicable absorbing
solution blank, /*g halide ion (Cl", Br~, F~)/ml,
not to exceed 1 /xg/ml which is 10 times the
published analytical detection limit of 0 . 1 /zg/ml
(It is also approximately 5 percent of the mass
concentration anticipated to result from a one
hour sample at 10 ppmv HCl . )
C = Concentration of hydrogen halide (HX) or halogen
(X2) , dry basis, mg/dscm.
triHx = Mass of HCl, HBr, or HF in sample, ug.
mX2 = Mass of C12 or Br2 in sample, ug.
Sx- = Analysis of sample, ug halide ion (Cl', Br~, F"
Vs = Volume of filtered and diluted sample, ml.
8.2 Average Dry Gas Meter Temperature and Average Orifice
Pressure Drop. See data sheet (Figure 5-2 of Method 5) .
8.3 Dry Gas Volume. Calculate Vro(std) and adjust for
leakage, if necessary, using the equation in Section 6.3 of
Method 5.
8.4 Volume of Water Vapor and Moisture Content. Calculate
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the volume of water vapor Vw(std) and moisture content Bws from the
data obtained in this method (Figure 5-2 of Method 5); use
Equations 5-2 and 5-3 of Method 5.
8.5 Isokinetic Variation and Acceptable Results. Use
Method 5, Sections 6.11 and 6.12.
8.6 Acetone Blank Concentration, Acetone Wash Blank Residue
Weight, Particulate Weight, and Particulate Concentration. For
particulate determination.
8.7 Total ng HC1, HBr, or HF Per Sample.
mm = K Vs (Sx- - Bx-) Eq. 26A-4
where: KHCi = 1.028 (/xg HCl//xg-mole) / (fig CI-/fig-mole) .
K^ = 1.013 (jig HBr//xg-mole)/ (p.
KHF = 1.053 (fig HF//xg-mole) / (/xg
8.8 Total ng Cla or Br2 Per Sample.
mX2 = Vs (Sx- - Bx-) Eq. 26A-5
8.9 Concentration of Hydrogen Halide or Halogen in Flue
Gas.
C = K mHx.B/V.ctd) Eq. 26A-6
where: K = 10'3 mg/^g
8.10 Stack Gas Velocity and Volumetric Flow Rate.
Calculate the average stack gas velocity and volumetric flow
rate, if needed, using data obtained in this method and the
equations in Sections 5.2 and 5.3 of Method 2.
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9. BIBLIOGRAPHY
1. Steinsberger, S. C. and J. H. Margeson. Laboratory-and
Field Evaluation of a Methodology for Determination of Hydrogen
Chloride Emissions from Municipal and Hazardous Waste
Incinerators. U.S. Environmental Protection Agency, Office of
Research and Development. Publication No. 600/3-89/064.
April 1989. Available from National Technical Information
Service, Springfield, VA 22161 as PB89220586/AS.
2. State of California Air Resources Board. Method 421 -
*
Determination of Hydrochloric Acid Emissions from Stationary
Sources. March 18, 1987.
3. Cheney, J.L. and C.R. Fortune. Improvements in the
Methodology for Measuring Hydrochloric Acid in Combustion Source
Emissions. J. Environ. Sci. Health. AJL9_(3): 337-350. 1984.
4. Stern, D.A., B.M. Myatt, J.F. Lachowski, and K.T.
McGregor. Speciation of Halogen and Hydrogen Halide Compounds in
Gaseous Emissions. In: Incineration and Treatment of Hazardous
Waste: Proceedings of the 9th Annual Research Symposium,
Cincinnati, Ohio, May 2-4, 1983. Publication No. 600/9-84-015.
July 1984. Available from National Technical Information
Service, Springfield, VA 22161 as PB84-234525.
5. Holm, R.D. and S.A. Barksdale. Analysis of Anions in
Combustion Products. In: Ion Chromatographic Analysis of
-------
Environmental Pollutants, E. Sawicki, J.D. Mulik, and
E. Wittgenstein (eds.). Ann Arbor, Michigan, Ann Arbor Science
Publishers. 1978. pp. 99-110.
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Appendix G.8
EPA Proposed Method 322
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(PROPOSED) TEST METHOD 322 -MEASUREMENT OF HYDROGEN CHLORIDE
EMISSIONS FROM PORTLAND CEMENT KILNS BY GFCIR
1.0 Applicability and Principle
1.1 Applicability. This method is applicable to the
determination of hydrogen chloride (HC1) concentrations in
emissions from portland cement kilns. This is an instrumental
method for the measurement of HC1 using an extractive sampling
system and an infrared (IR) gas-filter correlation (GFC)
analyzer. This method is intended to provide the cement industry
with a direct interface instrumental method. A procedure for
analyte spiking is included for quality assurance. This method
is considered to be self-validating provided that the
requirements in section 9 of this method are followed.
1.2 Principle. A gas sample is continuously extracted from
a stack or duct over the test period using either a source-level
hot/wet extractive subsystem or a dilution extractive subsystem.
A nondispersive infrared gas filter correlation (NDIR-GFC)
analyzer is specified for the measurement of HC1 in the sample.
The total measurement system is comprised of the extractive
subsystem, the analyzer, and the data acquisition subsystem.
Test system performance specifications are included in this
method to provide for the collection of accurate, reproducible
data.
1.3 Test System Operating Range. The measurement range
(span) of the test system shall include the anticipated HC1
concentrations of the effluent and spiked samples. The range
should be selected so that the average of the effluent
measurements is between 25 and 75 percent of span. If at any
time during a test run, the effluent concentration exceeds the
span value of the test system, the run shall be considered
invalid.
2.0 Summary of Method
2.1 Sampling and Analysis. Kiln gas is continuously
extracted from the stack or duct using either a source level,
hot/wet extractive system, or an in-situ dilution probe or heated
out-of-stack dilution system. The sample is then directed by a
heated sample line maintained above 350°F to a GFC analyzer
having a range appropriate to the type of sampling system. The
gas filter correlation analyzer incorporates a gas cell filled
with HC1. This gas cell is periodically moved into the path of
an infrared measurement beam of the instrument to filter out
essentially all of the HC1 absorption wavelengths. Spectral
filtering provides a reference from which the HC1 concentration
of the sample can be determined. Interferences are minimized in
the. analyzer by choosing a spectral band over which compounds
such as CO2 and H2O either do not absorb significantly or do not
match the spectral pattern of the HC1 infrared absorption.
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2.2 Operator Requirements. The analyst must be familiar
with the specifications and test procedures of this method and
follow them in order to obtain reproducible and accurate data.
3.0 Definitions
3.1 Measurement System. The total equipment required for
the determination of gas concentration. The measurement system
consists of the following major subsystems:
3.1.1 Sample Interface. That portion of a system used for
one or more of the following: sample acquisition, sample
transport, sample conditioning, or protection of the analyzers
from the effects of the stack gas.
3.1.2 Gas Analyzer. That portion of the system that senses
the gas to be measured and generates an output proportional to
its concentration.
3.1.3 Data Recorder. A strip chart recorder, analog
computer, or digital recorder for recording measurement data from
the analyzer output.
3.2 Span. The upper limit of the gas concentration
measurement range displayed on the data recorder.
3.3 Calibration Gas. A known concentration of a gas in an
appropriate diluent gas (i.e., N2) .
3.4 Analyzer Calibration Error. .The difference between the
gas concentration exhibited by the gas analyzer and the known
concentration of the calibration gas when the calibration gas is
introduced directly to the analyzer.
3.5 Sampling System Bias. The sampling system bias is the
difference between the gas concentrations exhibited by the
measurement system when a known concentration gas is introduced
at the outlet of the sampling probe and the known value of the
calibration gas.
3.6 Response Time. The amount of time required for the
measurement system to display 95 percent of a step change in gas
concentration on the data recorder.
3.7 Calibration Curve. A graph or other systematic method
of establishing the relationship between the analyzer response '
and the actual gas concentration introduced to the analyzer.
3.8 Linearity. The linear response of the analyzer or test
system to known calibration inputs covering the concentration
range of the system.
3.9 Interference Rejection. The ability of the system to
reject the effect of interferences in the analytical measurement
processes of the test system.
4.0 Interferences
4.1 Sampling System Interferences. An important
consideration in measuring HC1 using an extractive measurement
system is to ensure that a representative kiln gas sample is
delivered to the gas analyzer. A sampling system interferant is
a factor that inhibits an analyte from reaching the analytical
instrumentation. Condensed water vapor is a strong sampling
system interferant for HC1 and other water soluble compounds.
-------
"Cold spots" in the sampling system can allow water vapor in the
sample to condense resulting in removal of HC1 from the sample
stream. The extent of HC1 sampling system bias depends on
concentrations of potential interferants, moisture content of the
gas stream, temperature of the gas stream, temperature of
sampling system components, sample flow rate, and reactivity of
HC1 with other species in the gas stream. For measuring HC1 in a
wet gas stream, the temperatures of the gas stream and sampling
system components and the sample flow rate are of primary
importance. In order to prevent problems with condensation in
the sampling system, these parameters must be closely monitored.
4.1.1 System Calibration Checks. Performing these
calibration checks where HC1 calibration gas is injected through
the entire system both before and after each test run
demonstrates the integrity of the sampling system and capability
of the analyzer for measuring this water soluble and otherwise
unstable compound under ideal conditions (i.e., HC1 in N2) .
4.1.2 Analyte Spiking Checks. For analyte spiking checks,
HC1 calibration gas is quantitatively added to the sample stream
at a point upstream of the particulate filter and all other
sample handling components both before and after each test run.
The volume of HC1 spike gas should not exceed 10 percent of the
total sample volume so that the sample matrix is relatively
unaffected. Successfully performing these checks demonstrates
the integrity of the sampling system for measuring this water
soluble and reactive compound under actual sample matrix
conditions. Successfully performing these checks also
demonstrates the adequacy of the interference rejection
capability of the analyzer. (See section 9.3 of this method.)
4.2 Analytical Interferences. Analytical interferences are
reduced by the GFC spectroscopic technique required by the
method. The accuracy of HC1 measurements provided by some GFC
analyzers is known to be sensitive to the moisture content of the
sample. This must be taken into account in order to acquire
accurate results. These analyzers must be calibrated for the
specific moisture content of the samples.
5.0 Safety
This method may involve sampling at locations having high
positive or negative pressures, or high concentrations of
hazardous or toxic pollutants, and cannot address all safety
problems encountered under these diverse sampling conditions. It
is the responsibility of the tester(s) to ensure proper safety
and health practices, and to determine the applicability of
regulatory limitations before performing this test method.
Because HC1 is a respiratory irritant, it is advisable to limit
exposure to this compound.
6.0. Equipment and Supplies
Note: Mention of company or product names does not
constitute endorsement by the U. S. Environmental Protection
Agency.
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6.1 Measurement System. Use any GFC measurement system for
HC1 that meets the specifications of this method. All sampling
system components must be maintained above the kiln gas
temperature, when possible, or at least 350°F. The length of
sample transport line should be minimized and sampling rate
should be as high as possible to minimize adsorption of HC1. The
essential components of the measurement system are described in
sections 6.1.1 through 6.1.12.
6.1.1 Sample Probe. Glass, stainless steel, Hastalloy"1, or
equivalent, of sufficient length to traverse the sample points.
The sampling probe shall be heated to a minimum of 350°F to
prevent condensation. Dilution extractive systems must use a
dilution ratio such that the average diluted concentrations are
between 25 to 75 percent of the selected measurement range of the
analyzer.
6.1.2 Calibration Valve Assembly. Use a heated, three-way
valve assembly, or equivalent, for selecting either sample gas or
introducing calibration gases to the measurement system or
introducing analyte spikes into the measurement system at the
outlet of the sampling probe before the primary particulate
filter.
6.1.3 Particulate Filter. A coarse filter or other device
may be placed at the inlet of the probe for removal of large
particulate (10 microns or greater). A heated (Balston® or
equivalent) filter rated at 1 micron is necessary for primary
particulate removal, and shall be placed immediately after the
heated probe. The filter/filter holder shall be maintained at
350°F or a higher temperature. Additional filters at the inlet
of the gas analyzer may be used to prevent accumulation of
particulate material in the measurement system and extend the
useful life of components. All filters shall be fabricated of
materials that are nonreactive with HC1. Some types of glass
filters are known to react with HC1.
6.1.4 Sample Transport Lines. Stainless steel or
polytetrafluoroethylene (PTFE) tubing shall be heated to a
minimum temperature of 350°F (sufficient to prevent condensation
and to prevent HC1 and NH3 from combining into ammonium chloride
in the sampling system) to transport the sample gas to the gas
analyzer.
6.1.5 Sample Pump. Use a leak-free pump to pull the sample
gas through the system at a flow rate sufficient to minimize the
response time of the measurement system. The pump components
that contact the sample must be heated to a temperature greater
than 350°F and must be constructed of a material that is
nonreactive to HC1.
6.1.6 Sample Flow Rate Control. A sample flow rate control
valve and rotameter, or equivalent, must be used to maintain a
constant sampling rate within ±10 percent. These components must
be heated to a temperature greater than 350°F. (Hoifi: The
tester may elect to install a back-pressure regulator to maintain
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the sample gas manifold at a constant pressure in order to
protect the analyzer(s) from over-pressurization, and to minimize
the need for flow rate adjustments.)
6.1.7 Sample Gas Manifold. A sample gas manifold, heated
to a minimum of 350°F, is used to divert a portion of the sample
gas stream to the analyzer and the remainder to the by-pass
discharge vent. The sample gas manifold should also include
provisions for introducing calibration gases directly to the
analyzer. The manifold must be constructed of material that is
nonreactive to the gas being sampled.
6.1.8 Gas Analyzer. Use a nondispersive infrared analyzer
utilizing the gas filter correlation technique to determine HC1
concentrations. The analyzer shall meet the applicable
performance specifications of section 8.0 of this method. (Note:
Housing the analyzer in a clean, thermally-stable, vibration free
environment will minimize drift in the analyzer calibration.)
The analyzer (system) shall be designed so that the response of a
known calibration input shall not deviate by more than ±3 percent
from the expected value. The analyzer or measurement system
manufacturer may provide documentation that the instrument meets
this design requirement. Alternatively, a known concentration
gas standard and calibration dilution system meeting the
requirements of Method 205 of appendix M to part 51 of this
chapter, "Verification of Gas Dilution Systems for Field
Calibrations" (or equivalent procedure), may be used to develop a
multi-point calibration curve over the measurement range of the
analyzer.
6.1.9 Gas Regulators. Single stage regulator with cross
purge assembly that is used to purge the CGA fitting and
regulator before and after use. (This purge is necessary to
clear the calibration gas delivery system of ambient water vapor
after the initial connection is made, or after cylinder
changeover, and will extend the life of the regulator.) Wetted
parts are 316 stainless steel to handle corrosive gases.
6.1.10 Data Recorder. A strip chart recorder, analog
computer, or digital recorder, for recording measurement data.
The data recorder resolution (i.e., readability) shall be 0.5
percent of span. Alternatively, a digital or analog meter having
a resolution of 0.5 percent of span may be used to obtain the
analyzer responses and the readings may be recorded manually. If
this alternative is used, the readings shall be obtained at
equally-spaced intervals over the duration of the sampling run.
For sampling run durations of less than 1 hour, measurements at
1-minute intervals or a minimum of 30 measurements, whichever is
less restrictive, shall be obtained. For sampling run durations
greater than 1 hour, measurements at 2-minute intervals or a
minimum of 96 measurements, whichever is less restrictive, shall
be obtained.
6.1.11 Mass Flow Meters/Controllers. A mass flow meter
having the appropriate calibrated range and a stated accuracy of
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±2 percent of the measurement range is used to measure the HC1
spike flow rate. This device must be calibrated with the major
component of the calibration spike gas (e.g., nitrogen) using an
NIST traceable bubble meter or equivalent. When spiking HCl,. the
mass flow meter/controller should be thoroughly purged before and
after introduction of the gas to prevent corrosion of the
interior parts.
6.1.12 System Flow Measurement. A measurement device or
procedure to determine the total flow rate of sample gas within
the measurement system. A rotameter, or mass flow meter
calibrated relative to a laboratory standard to within ±2 percent
of the measurement value at the actual operating temperature,
moisture content, and sample composition (molecular weight) is
acceptable. A system which ensures that the total sample flow
rate is constant within ±2 percent and which relies on an
intermittent measurement of the actual flow rate
(e.g., calibrated gas meter) is also acceptable.
6.2 HC1 Calibration .Gases. The calibration gases for the
gas analyzer shall be HC1 in N2. Use at least three calibration
gases as specified below:
6.2.1 High-Range Gas. Concentration equivalent to 80 to
100 percent of the span.
6.2.2 Mid-Range Gas. Concentration equivalent to 40 to 60
percent of the span.
6.2.3 Zero Gas. Concentration of less than 0.25 percent of
the span. Purified ambient air may be used for the zero gas by
passing air through a charcoal filter or through one or more
impingers containing a solution of 3 percent H2O2.
6.2.4 Spike Gas. A calibration gas of known concentration
(typically 100 to 200 ppm) used for analyte spikes in accordance
with the requirements of section 9.3 of this method.
7.0 Reagents and Standards
7.1 Hydrogen Chloride. Hydrogen Chloride is a reactive gas
and is available in steel cylinders from various commercial gas
vendors. The stability is such that it.is not possible to
purchase a cylinder mixture whose HCl concentration can be
certified at better than ±5 percent. The stability of the
cylinder may be monitored over time by periodically analyzing
cylinder samples. The cylinder gas concentration must be
verified within 1 month prior to the use of the calibration gas.
Due to the relatively high uncertainty of HCl calibration gas
values, difficulties may develop in meeting the performance
specifications if the mid-range and high-range calibration gases
are not consistent with each other. Where problems are
encountered, the consistency of the test gas standards may be
determined: (1) by comparing analyzer responses for the test
gases with the responses to additional certified calibration gas
standards, (2) by reanalysis of the calibration gases in
accordance with sections 7.2.1 or 7.2.2 of this method, or (3) by
other procedures subject to the approval of EPA.
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7.2 Calibration Gas Concentration Verification. There are
two alternatives for establishing the concentrations of
calibration gases. Alternative No. 1 is preferred.
7.2.1 Alternative No. 1. The value of the calibration
gases may be obtained from the vendor's certified analysis within
1 month prior to the test. Obtain a certification from the gas
manufacturer that identifies the analytical procedures and date
of certification.
7.2.2 Alternative No. 2. Perform triplicate analyses of
the gases using Method 26 of appendix A to part 60 of this
chapter. Obtain gas mixtures with a manufacturer's tolerance not
to exceed ±5 percent of the tag value. Within 1 month of the
field test, analyze each of the calibration gases in triplicate
using Method 26 of appendix A to part 60 of this chapter. The
tester must follow all of the procedures in Method 26 (e.g., use
midget impingers, heated Pallflex TX40H175 filter (TFE-glass
mat), etc. if this analysis is performed. Citation 3 in section
13 of this method describes procedures and techniques that may be
used for this analysis. Record the results on a data sheet.
Each of the individual HC1 analytical results for each
calibration gas shall be within 5 percent (or 5 ppm, whichever is
greater) of the triplicate set average; otherwise, discard the
entire set and repeat the triplicate analyses. If the average of
the triplicate analyses is within 5 percent of the calibration
gas manufacturer's cylinder tag value, use the tag value;
otherwise, conduct at least three additional analyses until the
results of six consecutive runs agree within 5 percent (or 5 ppm,
whichever is greater) of the average. Then use this average for
the cylinder value.
7.3 Calibration Gas Dilution Systems. Sample flow rates of"
approximately 15 L/miri are typical for extractive HCl measurement
systems. These flow rates coupled with response times of 15 to
30 minutes will result in consumption of large quantities of
calibration gases. The number of cylinders and amount of
calibration gas can be reduced by the use of a calibration gas
dilution system in accordance with Method 205 of appendix M to
part 51 of this chapter, "Verification of Gas Dilution Systems
for Field Instrument Calibrations." If this option is used, the
tester shall also introduce an undiluted calibration gas
approximating the effluent HCl concentration during the initial
calibration error test of the measurement system as a quality
assurance check.
8.0 Test System Performance Specifications
8.1 Analyzer Calibration Error. This error shall be less
than ±5 percent of the emission standard concentration or ±1
ppm,(whichever is greater) for zero, mid-, and high-range gases.
. 8.2 Sampling System Bias. This bias shall be less than
±7.5 percent of the emission standard concentration or ±1.5 ppm
(whichever is greater) for zero and mid-range gases.
8.3 Analyte Spike Recovery. This recovery shall be between
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70 to 130 percent of the expected concentration of spiked samples
calculated with the average of the before and after run spikes.
9.0 Sample Collection, Preservation, and Storage
9.1 Pretest. Perform the procedures of sections 9.1.1.
through 9.1.3.3 of this method before measurement of emissions
(procedures in section 9.2 of this method). It is important to
note that after a regulator is placed on an HC1 gas cylinder
valve, the regulator should be purged with dry N2 or dry
compressed air for approximately 10 minutes before initiating any
HC1 gas flow through the system. This purge is necessary to
remove any ambient water vapor from within the regulator and
calibration gas transport lines; the HC1 in the calibration gas
may react with this water vapor and increase system response
time. A purge of the system should also be performed at the
conclusion of a test day prior to removing the regulator from the
gas cylinder. Although the regulator wetted parts are corrosion
resistant, this will reduce the possibility of corrosion
developing within the regulator and extend the life of the
equipment.
9.1.1 Measurement System Preparation. Assemble the
measurement system by following the manufacturer's written
instructions for preparing and preconditioning the gas analyzer
and, as applicable, the other system components. Introduce the
calibration gases in any sequence, and make all necessary
adjustments to calibrate the analyzer and the data recorder. If
necessary, adjust the instrument for the specific moisture
content of the samples. Adjust system components to achieve
correct sampling rates.
9.1.2 Analyzer Calibration Error. Conduct the analyzer
calibration error check in the field by introducing calibration
gases to the measurement system at any point upstream of the gas
analyzer in accordance with sections 9.1.2.1 and 9.1.2.2 of this
method.
9.1.2.1 After the measurement system has been prepared for
use, introduce the zero, mid-range, and -high-range gases to the
analyzer. During this check, make no adjustments to the system
except those necessary to achieve the correct calibration gas
flow rate at the analyzer. Record the analyzer responses to each
calibration gas. Note: A calibration curve established prior to
the analyzer calibration error check may be used to convert the
analyzer response to the equivalent gas concentration introduced
to the analyzer. However, the same correction procedure shall be
used for all effluent and calibration measurements obtained
during the test.
9.1.2.2 The analyzer calibration error check shall be
considered invalid if the difference in gas concentration
displayed by the analyzer and the concentration of the
calibration gas exceeds ±5 percent of the emission standard
concentration or ±1 ppm, (whichever is greater) for the zero,
mid-, or high-range calibration gases. If an invalid calibration
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is exhibited, cross-check or recertify the calibration gases,
take corrective action, and repeat the analyzer calibration error
check until acceptable performance is achieved.
9.1.3 Sampling System Bias Check. For nondilution
extractive systems, perform the sampling system bias check by
introducing calibration gases either at the probe inlet or at a
calibration valve installed at the outlet of the sampling probe.
For dilution systems, calibration gases for both the analyzer
calibration error check and the sampling system bias check must
be introduced prior to the point of sample dilution. For
dilution and nondilution systems, a zero gas and either a mid-
range or high-range gas (whichever more closely approximates the
effluent concentration) shall be used for the sampling system
bias check.
9.1.3.1 Introduce the upscale calibration gas, and record
the gas concentration displayed by the analyzer. Then introduce
.zero gas, and record the gas concentration displayed by the
analyzer. During the sampling system bias check, operate the
system at the normal sampling rate, and make no adjustments to
the measurement system other than those necessary to achieve
proper calibration gas flow rates at the analyzer. Alternately
introduce the zero and upscale gases until a stable response is
achieved. The tester shall determine the measurement system
response time by observing the times required to achieve a stable
response for both the zero and upscale gases. Note the longer of
the two times and note the time required for the measurement
system to reach 95 percent of the step change in the effluent
concentration as the response time.
9.1.3.2 For nondilution systems, where the analyzer
calibration error test is performed by introducing gases directly
to the analyzer, the sampling system bias check shall be
considered invalid if the difference between the gas
concentrations displayed by the measurement system for the
sampling system bias check and the known gas concentration
standard exceeds ±7.5 percent of the emission standard or ±1.5
ppm, (whichever is greater) for either the zero or the upscale
calibration gases. If an invalid calibration is exhibited, take
corrective action, and repeat the sampling system bias check
until acceptable performance is achieved. If adjustment to the
analyzer is required, first repeat the analyzer calibration error
check, then repeat the sampling system bias check.
9.1.3.3 For dilution systems (and nondilution systems where
all calibration gases are introduced at the probe), the
comparison of the analyzer calibration error results and sampling
system bias check results is not meaningful. For these systems,
the sampling system bias check shall be considered invalid if the
difference between the gas concentrations displayed by the
analyzer and the actual gas concentrations exceed ±7.5 percent of
the emission standard or ±1.5 ppm, (whichever is greater) for
either the zero or the upscale calibration gases. If an invalid
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calibration is exhibited, take corrective action, and repeat the
sampling system bias check until acceptable performance is
achieved. If adjustment to the analyzer is required, first
repeat the analyzer calibration error check.
9.2 Emission Test Procedures
9.2.1 Selection of Sampling Site and Sampling Points.
Select a measurement site and sampling points using the same
criteria that are applicable to Method 26 of appendix A to part
60 of this chapter.
9.2.2 Sample Collection. Position the sampling probe at
the first measurement point, and begin sampling at the same rate
as used during the sampling system bias check. Maintain constant
rate sampling (i.e., ±10 percent) during the entire run. Field
test experience has shown that conditioning of the sample system
is necessary for approximately 1-hour prior to conducting the
first sample run. This conditioning period should be repeated
after particulate filters are replaced and at the beginning of
each new day or following any period when the sampling system is
inoperative. Experience has also shown that prior to adequate
conditioning of the system, the response to analyte spikes and/or
the change from an upscale calibration-gas to a representative
effluent measurement may be delayed by more than twice the normal
measurement system response time. It is recommended that the
analyte spikes (see section 9.3 of this method) be performed to
determine if the system is adequately conditioned. The sampling
system is ready for use when the time required for the
measurement system to equilibrate after a change from a
representative effluent measurement to a representative spiked
sample measurement approximates the calibration gas response time
observed in section 9.1.3.1 of this method.
9.2.3 Sample Duration. After completing the sampling
system bias checks and analyte spikes prior to a test run,
constant rate sampling of the effluent should begin. For each
run, use only those measurements obtained after all residual
response to calibration standards or spikes are eliminated-and
representative effluent measurements are displayed to determine
the average effluent concentration. At a minimum, this requires
that the response time of the measurement system has elapsed
before data are recorded for calculation of the average effluent
concentration. Sampling should be continuous for the duration of
the test run. The length of data collection should be at least
as long as required for sample collection by Method 26 of part 60
of this chapter. One hour sampling runs using this method have
provided reliable data for cement kilns.
9.2.4 Validation of Runs. Before and after each run, or if
adjustments are necessary for the measurement system during the
run, repeat the sampling system bias check procedure described in
section 9.1.3 of this method. (Make no adjustments to the
measurement system until after the drift checks are completed.)
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Record the analyzer's responses.
9.2.4.1 If the post-run sampling system bias for either the
zero or upscale calibration gas exceeds the sampling system bias
specification, then the run is considered invalid. Take
corrective action, and repeat both the analyzer calibration error
check procedure (section 9.1.2 of this method) and the sampling
system bias check procedure (section 9.1.3 of this method) before
repeating.the run. ,
9.2.4.2 If the post-run sampling system bias for both the
zero and upscale calibration gas are within the sampling system
bias specification, then construct two 2-point straight lines,
one using the pre-run zero and upscale check values and the other
using the post-run zero and upscale check values. Use the slopes
and y-intercepts of the two lines to calculate the gas
concentration for the run in accordance with equation 1 of this
method.
9.3 Analyte Spiking—Self-Validating Procedure. Use analyte
spiking to verify the effectiveness of the sampling system for
the.target compounds in the actual kiln gas matrix. Quality
assurance (QA) spiking should be performed before and after each
sample run. The spikes may be performed following the sampling
system bias checks (zero and mid-range system calibrations)
before each run in a series and also after the last run. The HCl
spike recovery should be within ±30 percent as calculated using
equations 1 and 2 of this method. Two general approaches are
applicable for the use of analyte spiking to validate a GFC HCl
measurement system: (1) two independent measurement systems can
be operated concurrently with analyte spikes introduced to one of
the systems, or (2) a single measurement system can be used to
analyze consecutively, spiked and unspiked samples in an
alternating fashion. The two-system approach is similar to
Method 301 of this appendix and the measurement bias is
determined from the difference in the paired concurrent
measurements relative to the amount of HCl spike added to the
spiked system. The two-system approach must employ identical
sampling systems and analyzers and both measurement systems
should be calibrated using the same mid- and high-range
calibration standards. The two-system approach should be largely
unaffected by temporal variations in the effluent concentrations
if both measurement systems achieve the same calibration
responses and both systems have the same response times. (See
Method 301 of this appendix for appropriate calculation
procedures.) The single measurement system approach is
applicable when the concentration of HCl in the source does not
vary substantially during the period of the test. Since the
approach depends on the comparison of consecutive spiked and
unspiked samples, temporal variations in the effluent HCl
concentrations will introduce errors in determining the expected
concentration of the spiked samples. If the effluent HCl
concentrations vary by more than ±10 percent (or ±5 ppm,
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whichever is greater) during the time required to obtain and
equilibrate a new sample (system response time), it may be
necessary to: (1) use a dual sampling system approach,
(2) postpone testing until stable emission concentrations are
achieved, (3) switch to the two-system approach [if possible] or,
(4) rely on alternative QA/QC procedures. The dual-sampling
system alternative uses two sampling lines to convey sample to
the gas distribution manifold. One of the sample lines is used
to continuously extract unspiked kiln gas from the source. The
other sample line serves as the analyte spike line. One GFC
analyzer can be used to alternately measure the HC1 concentration
from the two sampling systems with the need to purge only the
components between the common manifold and the analyzer. This
minimizes the time required to acquire an equilibrated sample of
spiked or unspiked kiln gas. If the source varies by more than
±10 percent or ±5 ppm, (whichever is greater) during the time it
takes to switch from the unspiked sample line to the spiked
sample line, then the dual-sampling system alternative approach
is not applicable. As a last option, (where no other
alternatives can be used) a humidified nitrogen stream may be
generated in the field which approximates the moisture content of
the kiln gas. Analyte spiking into this humidified stream can be
employed to assure that the sampling system is adequate for
transporting the HC1 to the GFC analyzer and that the analyzer's
water interference rejection is adequate.
9.3.1 Spike Gas Concentration and Spike Ratio. The volume
of HC1 spike gas should not exceed 10 percent of the total sample
volume (i.e., spike to total sample ratio of 1:10) to ensure that
the sample matrix is relatively unaffected. An ideal spike
concentration should approximate the native effluent
concentration, thus the spiked sample concentrations would
represent approximately twice the native effluent concentrations.
The ideal spike concentration may not be achieved because the
native HC1 concentration cannot be accurately predicted prior to
the field test, and limited calibration -gas standards will be
available during the field test. Some flexibility is available
by varying the spike ratio over the range from 1:10 to 1:20.
Practical constraints must be applied to allow the tester to
spike at an anticipated concentration. Thus, the tester may use
a 100 ppm calibration gas and a spike ratio of 1:10 as default
values where information regarding the expected HC1 effluent
concentration is not available prior to the tests.
Alternatively, the tester may select another calibration gas
standard and/or lower spike ratio (e.g., 1:20) to more closely
approximate the effluent HC1 concentration.
9.3.2 Spike Procedure. Introduce the HC1 spike gas mixture
at a constant flow rate (±2 percent) at less than 10 percent of
the total sample flow rate. (For example, introduce the HC1
spike gas at 1 L/min (±20 cc/min) into a total sample flow rate
of 10 L/min). The spike gas must be preheated before
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introduction into the sample matrix to prevent a localized
condensation of the gas stream at the spike introduction point.
A heated sample transport line(s) containing multiple transport
tubes within the heated bundle may be used to spike gas up
through the sampling system to the spike introduction point. Use
a calibrated flow device (e.g., mass flow meter/controller) to
monitor the spike flow rate. Use a calibrated flow device (e.g.,
rotameter, mass flow meter, orifice meter, or other method) to
monitor the total sample flow-rate. Calculate the spike ratio
from the measurements of spike flow and total flow. (See
equation 2 and 3 in section 10.2 of this method.)
9.3.3 Analyte Spiking. Determine the approximate effluent
HC1 concentrations by examination of preliminary samples. For
single-system approaches, determine whether the HC1 concentration
varies significantly with time by comparing consecutive samples
for the period of time corresponding to at least twice the system
response time. (For analyzers without sample averaging, estimate
average values for two to .five minute periods by observing the
instrument display or data recorder output.) If the concentration
of the individual samples varies by more than ±10 percent
relative to the mean value or ±5 ppm, (whichever is greater), an
alternate approach may be needed.
9.3.3.1 Adjust the spike flow rate to the appropriate level
relative to the total flow by metering spike gas through a
calibrated mass flow meter or controller. Allow spike flow to
equilibrate within the sampling system for at least the
measurement system response time and a steady response to the
spike gas is observed before recording response to the spiked gas
sample. Next, terminate the spike gas flow and allow the
measurement system to sample only the effluent. After the
measurement system response time has elapsed and representative
effluent measurements are obtained, record the effluent unspiked
concentration. Immediately calculate the spike recovery.
9.3.3.2 If the spike recovery is not within acceptable
limits and a change in the effluent concentration is suspected as
the cause for exceeding the recovery limit, repeat the analyte
spike procedure without making any adjustments to the analyzer or
sampling system. If the second spike recovery falls within the
recovery limits, disregard the first attempt and record the
results of the second spike.
9.3:3.3 Analyte spikes must be performed before and after
each test run. Sampling system bias checks must also be
performed before and after each test run. Depending on the
particular sampling strategy and other constraints, it may be
necessary to compare effluent data either immediately before or
immediately after the spike sample to determine the spike
recovery. Either method is acceptable provided a consistent
approach is used for the test program. The average spike
recovery for the pre- and post-run spikes shall be used to
determine if spike recovery is between 70 and 130 percent.
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10.0 Data Analysis and Emission Calculations
The average gas effluent concentration is determined from
the average gas concentration displayed by the gas analyzer and
is adjusted for the zero and upscale sampling system bias checks,
as determined in accordance with section 9.2.3 of this method.
The average gas concentration displayed by the analyzer may be
determined by integration of the area under the curve for chart
recorders, or by averaging all of the effluent measurements.
Alternatively, the average may be calculated from measurements
recorded at equally spaced intervals over the entire duration of
the run. For sampling run durations of less than 1-hour, average
measurements at 2-minute intervals or less, shall be used. For
sampling run durations greater than 1-hour, measurements at 2-
minute intervals or a minimum of 96 measurements, whichever is
less restrictive, shall be used. Calculate the effluent gas
concentration using equation 1.
(<: - h ) 1 (Eq. 1)
\ HVK ^ _i_X\* -j- I* \
m* **" nrif ) ———-^—•-^—^— v^i *V )
i I fif\
. Q _ I c J where:
888 2 bc = Y-
intercept of
the
calibration
least-
squares
line.
bf = Y-intercept of the final bias check 2-point line.
bi = Y-intercept of the initial bias check 2-point
line.
Cgaa = Effluent gas concentration, as measured, ppm.
Cavg = Average gas concentration indicated by gas
analyzer, as measured, ppm.
mc = Slope of the calibration least-squares line.
mf = Slope of the final bias check 2-point line.
mt . Slope of the initial bias check 2-point line. -
The following equations are used to determine the percent
recovery (%R) for analyte spiking:
%R = (SM/CE) x 100 (Eq. 2)
where:
SM = Mean concentration of duplicate analyte spiked
samples (observed).
CE - Expected concentration of analyte spiked samples
(theoretical).
CE = CS(QS/QT) + SU(1-QS/QT) (Eq. 3)
where:
Cs - Concentration of HC1 spike gas (cylinder tag
value).
Qs = Spike gas flow rate.
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QT = Total sample flow rate (effluent sample flow plus
spike flow).
Su = Native concentration of HC1 in unspiked effluent
samples.
Acceptable recoveries for analyte spiking are ±30 percent.
11.0 Pollution Prevention
Gas extracted from the source and analyzed or vented from
the system manifold shall be either scrubbed, exhausted back into
the stack, or discharged into the atmosphere where suitable
dilution can occur to prevent harm to personnel health and
welfare or plant or personal property.
12.0 Waste Management
Gas standards of HC1 are handled as according to the
instructions enclosed with the materials safety data sheets.
13.0 References
1'. Peeler, J.W., Summary Letter Report to Ann Dougherty,
Portland Cement Association, June 20, 1996.
2. Test Protocol, Determination of Hydrogen Chloride
Emissions from Cement Kilns (Instrumental Analyzer Procedure)
Revision 4; June 20, 1996.
3. Westlin, Peter R. and John W. Brown. Methods for
Collecting and Analyzing Gas Cylinder Samples. Source Evaluation
Society Newsletter. 1(3):5-15. September 1978.
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